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UA-6 Absorbance Detector User Manual

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Contents

1. Wed SOZH Sled Tied 5072 944 822 1223 gocu BEZA peed 0224 soca LEZA 6124 Pon 9czu 8124 1200 m PES oosa 0624 6624 6824 6778 8604 Sn 01239 8723 1624 8823 9624 1804 Ler 5628 9824 TE 020 0 624 E N E ZEZA Bled gt o 14 9225 20241 6024 9021 8024 2 2029 7028 70214 sra ERA 020 eozn 1021 20014 1024 to ZOZH 027 8 S 7 6 nj al tint 0629 Za 6022 1079 072 1241 Q t7 zn 1022 A 4 UA 6 Detector Appendix A Replacement Parts REPLACEMENT DWG NO 60 0942 092 PART LIST MAIN SHEET 2 OF 2 CIRCUIT BOARD REV DATE 01120 PART NUMBER REFERENCE DESIGNATION DESCRIPTION 01 12 7520 00 C223 CAP 2 2uF 35VDC 202 119 0306 00 C229 CAP 100pF 600VDC 203 270 0013 00 0209 4011B 270 0103 01 U202 0213 IC TLO72ACP 205 270 0605 00 0201 0205 0204 4029B 206 270 1900 01 U205 539 270 1702 0
2. OF fi 0401 405 R401 2 OFFSET _ Rego 0409 410 R499 R500 3 R408 oe R440 R459 CR416 M R441 23 R409 R442 ME RTT RAT Rall 4022 R473 R412 C409 cag BE C435 76 419 R464 8465 i ses c J tier mE R468 F404 TN05 ne u TP404 TP406 CX R426 9 418 POWER CIRCUIT BOARD A 6 UA 6 Detector Appendix A Replacement Parts REPLACEMENT DWG NO 60 0942 093 PART LIST POWER SHEET 2 OF 3 laco int CIRCUIT BOARD REV B DATE 02070 I PART NUMBER REFERENCE DESIGNATION DESCRIPTION 401 110 6333 01 10428 C431 CAP 3300uF 50VDC 402 112 5050 00 416 CAP 10 0uF 20VDC 40 12 7520 00 C415 C432 C435 CAP 2 2uF 35VDC 119 0300 05 C408 CAP 3uF 100VDC 270 0015 00 0406 4011B 406 270 1105 00 0405 407 270 1107 00 0407 408 270 1900 01 0405 409 279 0020 00 0402 0404 410 279 0205 37 VR401 VR LM337 411 371 2014 80 R424 RES 1 40M 1 4W 1 412 371 2124 70 RES 1 24M 1 4W 1 413 371 2249 70 RES 2 49M 1 4W 1x 414 371 2332 70 R443 RES 3 32M 1 4W 1 415 371 2499 70 R426 R510 RES 4 99M 1 4W 1 3 404 405 74 2068 20 R463 RES 6 8 2W 1 377 4002 40 R449 R516 R523 RES 20 10W 10
3. Retriever 500 Retriever 500 fraction collector The information transmitted between the two units consists of tube change and rack change event marks RETRIEVER 500 PUMP VALVE 14 7 UA 6 DECTECTOR 8 0 e y m EJ TT CABLE 60 1020 217 Figure 3 12 Cable connection to the Retriever 500 3 14 Remote Chart Drive Control by Non Isco Equipment 3 18 The REMOTE CHART DRIVE jack is a polarized four pin jack that mates with a Cinch Jones S 304 CCT plug or equivalent The pins of the plug are 1 50 or 60 Hz time base at 19 VAC 2 common 3 pulse input 4 15 VDC This plug can be used to stop the chart drive motor or to drive the motor at a variable rate Connect a manual switch across pins 1 and 2 The chart drive stops when the switch is closed Short pins 1 and 2 The recorder chart motor may be driven with line frequency 60 Hz at 12 to 120 VAC across pins 3 and 4 TTL pulses may be used by placing an optoisolator between the TTL signal and pins 3 and 4 using the suggested circuit in Figure 3 13 6 Detector Section 3 Operation 5 3 e TTL SIGNAL 4 0 60 5 OPTO ISOLATOR Figure 3 13 Suggested Circuit for a Remote Chart Drive For a 60 Hz recorder chart travel will be 216000 recorder range cm hr pulses per cm For a 50 Hz recorder
4. N PRINTED SIDE OF PAPER TO REAR AND GUIDE BAR SPROCKET x PAPER HOLD DOWN AND GUIDE BAR PAPER GUIDE CUT CHART PAPER 5 SHOWN ABOVE CHART PAPER COMPARTMENT Figure 2 1 Recorder Chart Paper and Pen Installation 2 2 6 Detector Section 2 Preparation for Use 2 4 Attachment of the The optical unit is plugged into the UA 6 OPTICAL UNIT Optical Unit to the socket as shown in Figure 2 2 The optical unit can then be posi UA 6 tioned close to the column while the detector recorder component remains on the lab bench If the application calls for coldroom operation the optical unit can be placed inside the coldroom and the detector left outside by passing the optical unit cable through a port and completing the connection An optional 20 foot extension cable P N 68 1147 017 is available for applications which require additional separation of the optical unit and detector Each optical unit has a special mounting clamp which can be used to clamp to a ring stand or mast or by rotating the clamp 90 to the edge of a shelf 40 bear this label 33 5 Figure 2 2 Attaching an Optical Unit to the UA 6 M Note The optical unit should be mounted horizontally for proper operation 2 3 6 Detector Section 2 Preparation for Use 2 5 Changing The Type 11 optical unit is designed for wavelength detection Wavelengt
5. SEES 1 m zd 7 i 0 m 007 681 oBuey Q0 uBue puepeW 1 Af 39Nv8HOS8V 3O0NvH8HOSSV Figure 3 9 Absorbance Curves of Four Commonly Used Solvents 3 15 6 Detector Section Operation 3 12 2 Solvent Absorbance Absorbance curves for various buffers and organic solvents vary considerably as a function of wavelength so that some thought must be given to their choice Absorbance curves of four solvents commonly used in UV work are shown in Figure 3 9 Some sol vents such as tetrahydrofuran UV which begins absorbing shortly below 330 nm have a limited usefulness in this regard Others such as hexane UV remain relatively non absorbent down to 214 nm Note however that absorbance rises rapidly for most of these solvents below 214 nm 3 13 Connection to Other The interface cables available from Teledyne Isco for use with Instruments other instruments are summarized in Table 3 3 This table can be used as an ordering guide for cables The full catalog order number is listed in the table The cables are tagged with a seven digit number The input and output signals handled by the UA 6 and its rela tionship to other instruments in a system are shown in Figure 3 10 These instruments are typical of those that can be used with a UA 6 There are many cases though in which other instruments may be us
6. dWVv1 IL LSACAV I Figure 3 14 Problem Analysis Drift and Noise 3 20 6 Detector Section 3 Operation The following traces represent various difficulties as each is noted All were run with a chart speed of 1 5 and 3 cm hr with sensitivity at 0 01 AUFS unless otherwise noted DEFECTIVE MERCURY VAPOR LAMP OR BUBBLES IMPROPER CURRENT SETTING See Table 5 5 Item 2 0 1 AUFS With Preparative Flow Cell Note the sawtooth waveform NON Note abrupt shifts With HPLC Flow Cell Figure 3 15 Example Traces for Troubleshooting Analysis 3 21 6 Detector Section 3 Operation 3 22 UA 6 Detector Section 4 4 1 General Description 4 1 1 Optical Unit Figure 4 1 Optical Unit Light Path Theory of Operation N DANGER Risk of electric shock Disconnect the electric power before servicing Only trained service personnel may remove the case top Do not remove or disconnect earth ground bonding conductor A minimal monitoring system contains a Teledyne Isco optical unit and the UA 6 absorbance detector A fraction collector valve and whatever other equipment needed to collect samples or process optical data can be added as desired The optical unit contains a flow cell through which the liquid under inquiry moves a light source two filters and a pair of photosensors to detect optical activity The detector has all the necessary elec tronics to
7. j j j j j NOTE 1 This list is subject to chonge without notice A 24 UA 6 Detector Index A Applications for the UA 6 1 2 Baseline Adjustment 2 6 Bubble Formation and Retention 3 10 Cables 3 16 Calibration 2 6 Changing Wavelengths Type 11 2 4 Chart Paper and Pen 2 1 Chromatography Flow Cells 3 8 Circuitry Auto Baseline 4 3 Chart Recorder 4 7 Filtering 4 4 Gain 4 4 Lamp 4 5 Logarithmic Amplifier 4 4 Peak Separation 4 5 Power 4 6 Pulsing 4 5 Cleaning 5 20 Connecting to Other Instruments 3 16 Foxy 200 Fraction Collector 3 17 Remote Chart Drive 3 18 Controls and Connectors Rear Panel 1 7 Type 11 1 8 Controls and Indicators 1 2 Controls and Indicators Front Panel 1 5 F Filter Inspection 5 15 Flow Cells Applications 3 2 Descriptions 3 2 Installation 2 5 Front Panel 1 5 Fuses Type 12 2 4 Installation Chart and Pen 2 1 L Leakage Flow Cell Window 5 19 N Noise and Drift Minimizing 3 13 Noise Filter 3 11 o Optical Unit Attachment 2 2 Optical Units 1 1 P Peak Separator 3 12 4 5 Power 2 1 Problem Analysis 3 20 R Rear Panel 1 7 Replacement Recorder 5 1 Recorder Drive String 5 3 Regulating Photocell 5 13 Type 11 Lamp 5 11 Window or O Ring 5 18 Replacement Parts A 1 s Solvent Absorbance 3 16 T Technical Specifications 1 2 Theory of Operation Optical Unit 4
8. 6 Absorbance Detector Installation and Operation Guide TELEDYNE ISCO Everywhereyoulook Part 69 0943 266 of Assembly 60 0943 261 Copyright 1991 All rights reserved Teledyne Isco Revision M October 2013 Foreword This instruction manual is designed to help you gain a thorough understanding of the operation of the equipment Teledyne Isco recommends that you read this manual completely before placing the equipment in service Although Teledyne Isco designs reliability into all equipment there is always the possibility of a malfunction This manual may help in diagnosing and repairing the malfunction If a problem persists call or e mail the Teledyne Isco Technical Service Department for assistance Simple difficulties can often be diagnosed over the phone If it is necessary to return the equipment to the factory for service please follow the shipping instructions provided by the Customer Service Department including the use of the Return Authorization Number specified Be sure to include a note describing the malfunction This will aid in the prompt repair and return of the equipment Teledyne Isco welcomes suggestions that would improve the information presented in this manual or enhance the operation of the equipment itself Teledyne Isco is continually improving its products and reserves the right to change product specifications replacement parts schematics and instructions without notice Contact Infor
9. The date of Manufacture is in code within the serial number The first three numbers are the year of manufacture 207 is year 2007 followed by a letter for the month A is January B is February and so on Pump UA Monitor Hazmat Table 60 0943 269 Rev DECLARATION OF CONFORMITY ISM1 A Application of Council Directive 89 336 The EMC Directive 73 23 EEC The Low Voltage Directive Manufacturer s Name Teledyne Isco Inc Manufacturer s Address 4700 Superior Lincoln Nebraska 68504 USA Mailing Address P O Box 82531 Lincoln NE 68501 Equipment Type Environment Laboratory Equipment for Light Industrial Commercial Environments Trade Name Model No UA 6 with Type 11 amp 12 Optical Units Year of Issue 2000 Standards to which Conformity is Declared EN 61326 1998 EMC Requirements for Electrical Equipment for Measurement Control and Laboratory Use EN 61010 1 Safety Requirements for Electrical Equipment for Measurement Control and Laboratory Use Standard Description Severity Applied Performance Criteria EN61000 4 2 Electrostatic Discharge Level 2 4kV contact discharge B Level 3 8kV air discharge B EN61000 4 3 Radiated RF Immunity 80 MHz to 1000MHz 80 AM at 1kHz A Level 1 1 EN61000 4 4 Electrical Fast Transient Level 2 1kV on ac lines EN61000 4 5 Surge on AC Lines 1kV common mode 500V differential mode EN61000 4 6 Conducted RF on AC lines 150 kHz to 80 MHz B 3V rms 8096 modulated
10. a Move switch to INT b Remove the recorder top cover and tighten the set screws securing the 192 tooth gear to the feedback potentiometer shaft c Remove the recorder top cover and secure the pinion assembly to the DC motor shaft with Loctite 601 d Refer to Section 5 2 2 detector drive string installation See Figure 5 2 a The major remedies are as follows 1 Thoroughly clean the flow cell 2 Degas the buffer 3 Restrict the outlet to obtain head pressure on the flow cell 4 Restrict flow fluctuations by using a non reciprocating pump or a pulsation damper b Turn the optical unit COLDROOM HEATER switch to ON c Repair the leakage following the proce dure in Section 5 7 2 5 8 6 Detector Section 5 Maintenance and Adjustment Table 5 2 Recorder Troubleshooting Continued Problem 5 Recorder does not Event Mark at a fraction collector movement 6 Recorder does not return to the original baseline after a peak has passed and there is no light absorbing medium in the flow sys tem Probable Cause a Defective components in the detector Event Mark circuitry b Incorrect connection to the fraction collec tor a Incomplete flushing of the flow cell b Gradient elution Solution a Using standard electronic techniques repair or replace as required b Connect the detector to the fraction collec tor following the procedure in Section 3 13 a The maj
11. EN61000 4 11 Voltage Dips Short Interruptions 0 5 cycle each polarity 100 B CISPR11 RF Emissions Group 1 Class A Industrial Scientific and EN 55011 Medical Equipment EN61000 3 2 3 3 Harmonic Flicker Group1 Class A wj We the undersigned hereby declare that the design of the equipment specified above conforms to the above Directive s and Standards as of April 3 2000 William Foster USA Representative TELEDYNE ISCO A Teledyne Technologies Company William Foster Director of Engineering Teledyne Isco Inc 4700 Superior Street Lincoln Nebraska 68504 Phone 402 464 0231 Fax 402 464 4543 60 0942 121 RevE Teledyne Isco One Year Limited Factory Service Warranty This warranty exclusively covers Teledyne Isco instruments providing a one year limited warranty covering parts and labor Any instrument that fails during the warranty period due to faulty parts or workmanship will be repaired at the factory at no charge to the customer Teledyne Isco s exclusive liability is limited to repair or replacement of defective instruments Teledyne Isco is not liable for consequential damages Teledyne Isco will pay surface transportation charges both ways within the 48 contiguous United States if the instrument proves to be defective within 30 days of shipment Throughout the remainder of the warranty period the customer will pay to return the instrument t
12. Use of the 1 5 and 5 0 seconds rise time settings is highly rec ommended for peak separation in low pressure LC These set 6 Detector Section 3 Operation 3 10 Built in Chart Recorder 3 11 Built In Peak Separator 3 11 1 PEAK SEPARATOR Switch Figure 3 8 Sample Chromatogram 3 12 tings will help eliminate false peak cutting due to baseline and bubble noise The UA 6 has a built in recorder that provides a permanent record of chromatograms that can be conveniently taped in a lab notebook This paper is printed with a 10 cm wide grid strip with 2 mm minor and 1 cm major divisions Increasing absorbance causes the pen to deflect to the left The internal recorder in the UA 6 may be used as a stand alone recorder see Section 3 15 UA 6 detectors include a built in peak separator for collecting chromatography peaks with a fraction collector The peak sepa rator is a change of slope detector which cuts peaks based on the first derivative of the curve and not an absorbance threshold or level The peak separator is designed to collect all peaks regardless of their degree of resolution Peak cutting with the peak separator is largely automatic The PEAK SEPARATOR switch is used to fine tune peak cutting based on the expected peak widths at baseline The peak sepa rator can most accurately respond to baseline peak widths that range from 0 2 to 2 times the selected peak duration For peaks shorter than 0 2X the selected s
13. elis RAN Id 5 22 Appendix A Replacement Parts Replacement Parts 0 a suma VY dp Q WE 1 List of Figures 1 1 UA 6 Detector with Type 11 Optical Unit 1 2 xii Isco UA 6 Table of Contents 1 2 UA 6 Front Panel 1 5 1 3 UA 6 Rear 1 1 6 1 4 11 Controls and Connectors 1 8 2 1 Recorder Chart Paper and Pen Installation 2 2 2 2 Attaching an Optical Unit to the UA 6 2 3 2 3 Changing Wavelengths in the Type 11 Optical Unit 2 4 2 4 Changing the Source Screen in the Type 11 Optical Unit 2 5 2 5 Installing Flow Cells 2 6 3 1 Preparative Flow Cell 3 3 3 2 Flow Cell Cross Section 3 4 3 3 Flow Cell Flow Pressure Characteristics 3 5 3 4 Medium Pressure 400 psi 28 kg cm Lead Connector Installation 3 7 3 5 Lead Connector Assembly for High flow Rate Flow Cell 3 8 3 6 Ferrule Application Information 3 9 3 7 Effect of Noise Filter on Baseline Noise
14. 0 5 1 0 2 0 set lamp and optics Rotary selector switch Used to establish the full scale absorbance range Setlamp and optics This position overrides AUTO BASELINE and provides equal voltage to the opti cal unit photocells At this time the optical unit should be balanced It also initializes the lamp cur rent adjust circuit Type 11 only RECORDER OFFSET Rotary control Used for fine positioning of the absorbance baseline zero NOISE FILTER 0 5 1 5 5 0 3 position selector switch Reduces noise by employing a Bessel type active filter The 0 5 1 5 and 5 0 positions indicate the approximate theoretical response time in seconds for 10 to 90 percent full scale output deflection Standby Operate LED Indicator lamp Lights to indicate that secondary power is applied to circuitry and the unit is in operational status RED Type 11 lamp is warming up Red after warm up indicates lamp current needs to be reset GREEN Type 11 lamp current is proper ready for operation OPTICAL UNIT WARNING FRACTION COLLECTOR 8 mur re WARNING THIS INSTRUMENT IS EQUIPPED WITH INTERNAL HEATERS TO PREVENT CONDENSATION IN THE INSTRUMENT THE INSTRUMENT OUTLET FOR THE HEATERS TO OPERATE ABS UNIT REMOTE CHART DRIVE MUST PLUGGED INTO POWER RECORDER RECORDER REC INT EX
15. 2 1 Unpacking scence RET Sie bee Reed heed ee ee 2 1 2 2 Preparation for Use 2 1 2 3 Installing the Chart Paper and 2 1 2 4 Attachment of the Optical Unit to 6 2 3 2 5 Changing Wavelengths with the Type 11 Optical Unit 2 4 2 6 Installation of Flow Cells 1 4 2 5 2 7 Calibrating to an External 2 6 2 8 Baseline Adjustment for 2 6 Section 3 Operation 3 T Introduction ruan l ee 8 1 3 2 Flow Cell Applications 3 2 3 2 1 Preparative Flow Cells 68 0080 001 002 034 3 2 3 2 2 High Flow Rate Cell 68 0080 023 3 2 3 3 Flow Cell Descriptions 3 2 3 3 1 Preparative Flow Cells 3 3 3 3 2 High Flow Rate Cell 3 5 3 4 Flow Pressure Characteristics 3 6 3 5 Tubing Connections for Plastic Lead Connectors 3 6 3 6 Tubing Connections for High Flow Rate Cell 3 7 3 7 Selecting Chromatogra
16. 402 465 3022 E mail Iscolnfo teledyne com 1 Appendix Replacement Parts UA 6 Detector 9 LIND YAMOd 33S LIND NIVW 33S INaN39V1434 HOLIMS 04 9340934 33S 9IAU0934 335 2 UA 6 Detector Appendix A Replacement Parts REPLACEMENT PARTS LIST wo 60 0942 083 SHEET 2 OF 2 Isco Inc v DATE 91172 PART NUMBER DESCRIPTION 1 410 3308 00 SW DPDT SLIDE SIE G 55053350 BRI 2 POLE TI POS WOT SHOWN 8 2 POLE 6 FOS NOT SHOW s 8 025200 knoe weon OOOO S 36 BN SPDTFUSHBUTRN 7 Note 1 For current prices and quotations on parts contact Isco Service Department 800 228 4250 2 This list is subject to change without notice A 3 UA 6 Detector Appendix A Replacement Parts MAIN CIRCUIT BOARD 297 2760 6
17. PART NUMBER DESCRIPTION 69 0943 237 SPUR GEAR 60 1844 207 PULLEY ASSY TIMING BELT CHART PAPER 60 0947 020 RECORDER PEN PACKAGE OF 5 60 0614 022 MOTOR 55 60 0944 116 MOTOR 55 60 0943 258 24 FIBER CABLE 69 0945 255 SW 1 POLE 11 POS 250 0440 06 250 0440 08 PULLEY 205 2012 01 SPRING 60 0944 130 SWITCH HARNESS INCLUDES ITEM 10 Note 1 For current prices and quotations on parts contact Service Department 800 228 4250 2 This list is subject to change without notice A 10 9 9 e C5 C8 C10 UA 6 Detector Appendix Replacement Parts R23 DAMP R32 GAIN OTP3 OTP4 OTP5 SPAN ZERO R42 UA 6 Detector Appendix A Replacement Parts RECORDER CIRCUIT BOARD REV DATE 02182 PART NUMBER REFERENCE DESIGNATION 140 9004 13 m z DESCRIPTION CAP 15UF 25V CAP 10UF 35V TANT PLUG 10 PIN 156 PLUG 12 PIN 156 C6 C1 j 2 4 PLUG 12P 100 1 8 7 2 4 1 PLUG 8P 100 CONN 3PIN MT 4518 CNTR 143 3409 04 P5 P6 4081 AND GATE 250 0700 06 o 40018 3530 403 15 U U R 371 2014 80 24 RES 1 4 1 44 1 RES 25 5 25W 5x 1
18. the roller 5 Use the manual advance thumb wheel to help draw the paper the rest of the way around the roller 6 If the paper is feeding crooked pull the short side forward allow a few sprocket holes to tear as needed until the paper is feeding squarely Advance the paper until the full width of smooth paper has cleared the guide bar Be sure the sprockets are engaging the sprocket holes in the paper 7 Lay the supply roll of chart paper in the chart paper com partment under the roller If necessary rewind any unwound portion first 8 The paper can now be advanced either manually or auto matically 2 1 6 Detector Section 2 Preparation for Use M Note If the recorder has been sitting overnight tear off about three inches of chart paper to preclude the possibility of the paper rolling around the drum To install the pen refer to Figure 2 1 1 Slide the pen cartridge into its holder A dimpled clasp holds it in place 2 Remove the pen cap a press fit and lower the pen with the pen lift arm left of the roller to ready the pen for use Replace the pen cap on the pen when the recorder is not in use to prevent the tip from drying out 3 To remove the pen pull the cartridge straight out of the holder PEN LIFT BAIL ASSEMBLY 2 CARTRIDGE HOLDER ASSEMBLY PEN CARTRIDGE MANUAL milis ADVANCE WHEEL X PROTECTIVE PEN CAP PAPER HOLD DOWN J MANUAL PEN LIFT ARM
19. 1 Part Replacement u u shades eee Pusula ie S a Pah rude aS depen ot 5 1 5 2 1 Recorder Replacement 5 1 5 2 2 Recorder Drive String Installation 5 3 Timing Belt Tension Adjustment 5 4 Cleaning the 5 5 Troubleshooting 4 yel ek ee an 5 5 Type 11 Optical Unit Maintenance 5 11 5 6 1 11 UV Lamp Replacement 5 11 5 6 2 Regulating Photocell Assembly Replacement 5 13 5 6 3 Filter Assembly Inspection 5 15 5 6 4 Troubleshooting 5 15 Flow Cell Maintenance and 5 18 5 7 1 Window or O Ring Replacement 5 18 5 7 2 Correcting for Flow Cell Window 5 19 5 7 8 Troubleshooting 5 20 5 7 4 Flow Cell Cleaning Procedures 5 20 5 7 5 Cleaning the Back Pressure Regulator 5 21 5 7 6 Service 5 21 5 7 7 How to Ship Returns 5 21 5 1 8 Purchasing Parts 2 2 26 al
20. 1 UA 6 4 2 Timing Belt 5 4 Troubleshooting 3 20 5 5 Baseline 5 6 Flow Cells 5 20 General 5 10 Optical Units 5 15 Recorder 5 8 Tubing Connections High Flow Rate Cells 3 7 Plastic Lead Connectors 3 6 Type 11 Changing Wavelengths 2 4 Controls and Connectors 1 8 Index 1 UA 6 Detector Index Lamp Replacement 5 11 Theory of Operation 4 8 Type 12 Fuses 2 4 Index 2 Disregard the following Radio Interference Statement and Declara tion of Conformity if your instrument does not have a CE label on its rear panel Isco UA 6 RADIO INTERFERENCE STATEMENT FCC NOTE This equipment has been tested and found to comply with the limits for a Class A digital device pursuant to Part 15 of the FCC Rules These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment This equipment generates uses and can radiate radio frequency energy and if not installed and used in accordance with the instruction manual may cause harmful interference to radio communications Operation of this equipment in a residential area is likely to cause harmful interference in which case the user will be required to correct the interfer ence at his own expense Canada This ISM apparatus meets all requirements of the Canadian Interference Causing Equipment Regulations Ce g n rateur de fr quence radio ISM respecte toutes le
21. 3 11 3 8 Sample Chromatogram 3 12 3 9 Absorbance Curves of Four Commonly Used Solvents 3 15 3 10 Input and Output Signals of the 6 3 16 3 11 Cable Connection to the Foxy R1 or R2 3 17 3 12 Cable connection to the Retriever 500 3 18 3 13 Suggested Circuit for a Remote Chart Drive 3 19 3 14 Problem Analysis Drift and Noise 3 20 3 15 Example Traces for Troubleshooting Analysis 3 21 4 1 Optical Unit Light Path 4 1 4 2 UA 6 Detector Block Diagram 4 2 4 3 Type 11 Optical Unit Functional Diagram 4 9 4 4 Type 11 Optical Unit Schematic Diagram 4 10 4 5 11 Absorbance Detector Block Diagram 4 11 5 1 Built In Recorder Removal and Installation 5 2 5 2 Recorder String Routing 5 3 5 3 Timing Belt Tension Adjustment 5 5 5 4 UV Lamp and Regulating Photocell Removal and Installation 5 14 5 5 Window and O Ring Removal and Installation 5 19 List of Tables 1 1 Technical Specifi
22. 3 6 1 Ifthe flow cell has been disassembled for cleaning install the lead connector in the flow cell body and finger tighten 2 Slide the nut over the end of the tubing 3 Slide the ferrule over the end of the tubing Ensure that the larger diameter of the conical shaped ferrule is facing the nut 4 Insert the tubing into the lead connector and push the tub ing in until it bottoms out When using the red connector and 16inch OD tubing take care that the tubing does not pass through the end of the connector into the flow cell 5 Carefully engage the nut with the lead connector and screw the nut down until finger tight N CAUTION Finger tightening is sufficient Do not overtighten the lead con nector nut or allow the lead connector to turn This can result in extensive deformation of the plastic tubing The seal quality is assured through compression of the ferrule between the tubing and the conical section of the lead connector 6 Detector Section 3 Operation PLUMB THIS END TO MATCH THE OTHER nau LARGE BORE LEAD CONNECTOR 60 0643 254 red SMALL BORE LEAD CONNECTOR black 60 0923 013 optional POLYETHYLENE FERRULE 60 0923 017 D PREP FLOW CELL LEAD CONNECTOR beige 60 1853 034 A 1 16 POLYETHYLENE FERRULE 60 0083 163 NT HITTING 60 0923 015 Figure 3 4 Medium Pressure 400 psi 28 kg cm Lead Connector Installation 3
23. 374 400 0914 00 401 CR402 CR403 404 CR405 DIO 1N914 CR406 CR407 CR408 CR411 CR412 CR415 CR414 415 CR416 CR417 416 417 418 CR418 CR419 CR420 CR421 CR422 rr L L U U CR423 CR424 CR425 CR426 CRATE f CR428 CR429 CR430 m 9 400 2152 09 CR409 410 DIO 152378 420 8436 CR437 CR438 CR439 CR440 CR441 CR442 CR443 422 425 402 0237 02 0402 XSTR 203707 402 0240 00 0401 0404 XSTR 2N4058 411 0311 56 F402 FUSE 1 5A T 411 0322 42 401 F403 FUSE 75A F 427 60 0945 043 U401 IC SEL CA3160AE NOTE THIS LIST SUBJECT TO CHANGE WITHOUT NOTICE 2 gt NO s 7 UA 6 Detector Appendix A Replacement Parts REPLACEMENT DWG PART LIST SHEET 3 OF REV B DATE PART NUMBER REFERENCE DESIGNATION DESCRIPTION 400 0158 17 CR444 DIO 1 5817 411 0311 70 F404 FUSE 3A T 0 m 8 Inc NO ei L3 Ed Ea o 5 Tn E NOTE THIS LIST SUBJECT TO CHANGE WITHOUT NOTICE A 8 UA 6 Detector Appendix A Replacement Parts NN N N NN A 9 UA 6 Detector Appendix A Replacement Parts REPLACEMENT PARTS LIST 60 0942098 5 2 OF 2 Isco Inc REV A DATE 91318
24. 6 Tubing Connections The polypropylene lead connectors provided with the high flow for High Flow Rate rate flow cell will accommodate 3 8 inch OD and 1 4 inch OD Cell flexible or rigid plastic tubing The ferrule nut the ferrule and nut are all one piece are made of polypropylene as well To assemble these fittings to the flow cell body use the following procedure and refer to Figure 3 6 1 Push the tubing through the threaded ferrule nut 2 If 3 8 inch OD 1 4 inch ID flexible tubing is being used push the tubing insert into the end of the tubing 3 Insert the tubing into the lead connector and tighten the threaded ferrule nut N CAUTION Use only finger pressure to tighten the lead connector in the flow cell body during step 4 below Over tightening can result in extensive damage to the flow cell which would inhibit insertion of the spacer rods for pathlength adjustment on the variable pathlength flow cell 4 Thread the lead connector into the flow cell body using only finger pressure to tighten it when resistance is felt 3 7 6 Detector Section 3 Operation THREADED FERRULE NUT TUBING Figure 3 5 Lead Connector Assembly for High flow Rate Flow Cell TUBING INSERT FOR 3e OD X 14 FLEXIBLE TUBING FLOW CELL BODY LEAD CONNECTOR 3 7 Selecting Depending on the type of liquid chromatography method flow Chromatography cells with different internal configurations volumes and optical Fl
25. General Description 4 1 Optical Unitn cos gee Goh aks Deck 4 1 4 1 2 WA 6 Detector iss ine rate en ete as 4 2 Detailed 4 3 4 2 1 Auto Baseline Circuit 4 3 4 2 2 Logarithmic Amplifier 4 4 4 2 3 Gain Amplifiers 4 4 4 2 4 Noise Filtering 4 4 4 2 5 Recorder Offset Set Lamp and Optics 4 5 4 2 6 Peak 4 5 4 2 7 Injection and Event Mark 4 5 4 2 8 Lamp Brightness Regulator 4 5 4 2 9 Power Supply iei Les een C Dre 4 6 4 2 10 Built In Chart Recorder 4 4 2 11 eo nhan 4 7 11 Optical Unit Theory of Operation 4 8 ASA General u a oe ar e 4 8 4 3 2 Absorbance Detector Circuit 4 10 Section 5 Maintenance and Adjustment 5 1 5 2 5 3 5 4 5 5 5 6 5 7 Removal and Installation of the Case 5
26. Rate Cell Figure 5 5 Window and O Ring Removal and Installation 5 7 2 Correcting for Flow Cell Window Leakage The method for correcting leaks that may occur around the flow cell windows is presented in the following paragraphs This method is applicable to all flow cells 1 Remove the flow cell window using the procedures speci fied in section 5 7 1 steps 1 through 3 2 Inspect the O ring Figure 5 5 for signs of damage 3 If the O ring is damaged replace with a new one 4 If the O ring shows no signs of damage applicable to pre parative flow cells and high flow rate flow cells only apply a very small amount of fluorosilicone oil to the O ring N CAUTION Use the fluorosilicone oil sparingly and DO NOT get any on the window area that is in the light path Fluorosilicone oil absorbs UV light Fluorosilicone oil within the flow cell may cause air bubbles to adhere to the window and flow cell inner surfaces 5 Assemble the flow cell using the procedures specified in section 5 7 1 steps 4 through 8 5 19 6 Detector Section 5 Maintenance and Adjustment 5 7 3 Troubleshooting The most common malfunctions that may occur during normal operation of the flow cells are identified in Table 5 6 which iden tifies the problem probable cause and the solution Table 5 6 Flow Cell Troubleshooting Problem Probable Cause Solution 1 Leakage across the a O ring is damaged Figure 5 5 a Replace with a n
27. Specifications Pathlength mm 2 1 Illuminated Volume 15 3 7 Illuminated Volume per 75 75 37 cm light path Hold Up Volume 45 172 9 6 198 Part Number 68 0080 001 68 0080 002 68 0080 034 68 0080 023 Pressure Rating 200 psi 14 kg cm 200 psi 14 kg cm 400 psi 28 kg cm 200 psi 14 kg cm Tubing OD Accomodates 1 8 or Accomodates 1 8 or Accomodates 1 8 or Accomodates 3 8 or 1 16 inch steel 1 16 inch steel 1 16 inch steel 1 4 inch flexible or rigid plastic or glass plastic or glass plastic or glass plastic Standard O Ring Material Viton Viton EPR Viton Optional Replacement 202 3070 13 202 3070 13 202 2070 17 202 3070 13 O Rings Part 3 4 6 Detector Section 3 Operation 3 3 2 High Flow Rate Cell The high flow rate cell with a fixed pathlength 5 mm has the same construction as the preparative cells but has a sinch flow path This cell is capable of working with flow rates up to 3 liters per minute Compression fittings made of stainless steel and polypropylene are provided with the fixed pathlength flow cell and will accom modate 8 inch or 1 4 inch plastic tubing EN Imm SE 2 2 E ES SUCROSE WATER En a 5 Sa D I 1 t l 1 1 1 o I I 1 1 l 1 1 T 1 1 I 0 200 300 400 500 600 700 900 1000
28. alerta sobre la presencia de alto voltaje en el interior del producto gt Esta se al le advierte sobre la importancia de las instrucciones del manual que acompa an a este producto CAUTION LIQUIDS ASSOCIATED WITH THIS INSTRUMENT MAY BE CLASSIFIED AS CARCINOGENIC BIOHAZARD FLAMMABLE OR RADIOACTIVE SHOULD THESE LIQ UIDS BE USED IS HIGHLY RECOMMENDED THAT THIS APPLICATION BE ACCOMPLISHED IN AN ISO LATED ENVIRONMENT DESIGNED FOR THESE TYPES OF MATERIALS IN ACCORDANCE WITH FEDERAL STATE AND LOCAL REGULATORY LAWS AND IN COMPLIANCE WITH YOUR COMPANY S CHEMICAL HYGIENE PLAN IN THE EVENT OF A SPILL IN ALL CASES WHEN USING TELEDYNE ISCO INC INSTRU MENTATION PRUDENCE AND COMMON SENSE MUST BE USED CAUTION If this instrument is used in a manner not specified in this manual the protection provided by the equipment may be impaired vii viii AVIS LES LIQUIDES QUI SONT ANALYSES DANS CET INSTRU MENT PEUVENT ETRE CANCERIGENES HASARDS BIOLOGIQUES INFLAMMABLES OU RADIOACTIFS SI VOUS DEVEZ UTILISER CES LIQUIDES HASARDEUX IL EST TRES RECOMMAND QUE VOUS LE FAITES L INT RIEUR D UN ENVIRONNEMENT ISOL CONCU POUR TELS LIQUIDES CET ENVIRONNEMENT ISOL DEVRAIT TRE CONSTRUIT SELON LES 5 F D RAUX PROVINCIAUX ET LOCAUX AUSSI QUE LE PLAN DE VOTRE COMPAGNIE QUI CONCERNE L V NEMENT D UN ACCIDENT AVEC LES MATIERES HASARDEUSES EN TOUT CAS UTILISEZ TOUJ
29. chart travel will be 180000 recorder range cm hr pulses per cm 3 15 Converting the Switch the recessed rear panel switch INT EXT to external Internal Recorder for Connect external signal source to the red INT REC socket and Stand Alone the black common socket Operation 3 19 6 Detector Section 3 Operation NOILN3L 33 NOILVWHO4 3 88n8 NOISSNISIA 33S 1 sAIADAANI SI YY 315 1VidiM v9 A3LIINNOI LNOHLIM 51132 TIVISNI3H 9 NIN OZ 404 5 9 N3903LIIN ASQ 51132 MOTE 43040 LVHL NI XJLYM JNVX3H Vd 51132 NVID 19 39721 SI g JIVOSQIN LV Nad 43040934 39V1d OL 135330 343030238 JNITSSVEOLNV JSN v N3dO XVN OL LINN 40 80N3 3 1135 8 32 1 CV TVOILdO JHL JO SONIN3dO 3015110 ANOJ 3 0 3dvl 320 1 51132 3AOW3M IV 53 61132 3 ISN A 5 33 NOILVWHO4 S9NINS3ONOO NOISSNISIA 33S ON JNVX3H NYID 51142 014 WO3J NOILN31 33 SMOQNIM 3JAON33 72 3 NOU VW3OJ 3188na S9NINH3ONOO NOISSNOSIA 33S 4 9 5 53 ST139010Hd 13S an 33173 SAM ALINIIAIIA 3 SA ON ON 32 1434 MO FOWL SI NOILO3S 33S
30. control f Flow cell is dirty g Defective UV lamp in the optical unit h Defective filter cartridge in the optical unit i Defective photocell in the optical unit j Defective AUTO BASELINE switch in the detector k Defective RECORDER OFFSET control in the detector Defective recorder m Defective electronic components on the detector circuit boards a Recorder offset control out of adjustment a Install the required source screens and matching filters see Table 2 1 b Reverse the cell locations of the matched source screens and filters c Calibrate the detector following the proce dure in Section 2 7 d Switch to INTERNAL e Refer to the baseline procedure specified in Section 2 8 f Clean the flow cell following the procedure in Section 5 7 4 g Replace the UV lamp following the proce dure in Section 5 6 1 h Check the filter cartridge following the pro cedure in Section 5 6 3 and if required replace it with a serviceable one i Return optical unit to Teledyne Isco for photocell replacement j Replace switch k Replace the recorder offset control Replace following the procedure in Section 5 2 1 or repair as required m Repair or replace components as required An electronic technician should check the circuit boards using standard test procedures a Set recorder offset control to the center mark 5 6 6 Detector Section 5 Mainte
31. from the photocell and filter holders and with the optical unit turned ON held up to the aperture in the reflector plate with the flanged end of the filter assembly towards the light source The filter assembly can be visually inspected by sighting through the opposite end and viewing the color emissions Source screens matching the filter assembly wavelengths must be installed in the optical unit for these inspection procedures The filter assemblies are listed numerically in Table 5 4 and the resultant color emissions are identified against each filter with the defects necessitating replacement of the filter presented in the adjacent column N CAUTION Do not disassemble the filter assemblies This can result in damage to the filter which will require replacement of the whole assembly M Note The 254 nm through 365 nm filter assemblies can be checked using the light source of the Type 11 optical unit in a semi dark room The most common malfunctions that may occur during normal operation of the optical unit are identified in Table 5 5 which lists the problem probable cause and the solution 6 Detector Section 5 Maintenance and Adjustment Table 5 4 Filter Assembly Inspection Wavelength nm Serviceable Indication Defective Indication a Dim but uniform green or yellowish green a Uneven glow very dim glow dark spots or glow cracks b Same as item a but dimmer b Same as item a c Same as item a but m
32. initial pressure M Note A one meter length of 0 005 inch ID stainless steel tubing will provide a back pressure of approximately 75 psig at a flow rate of 0 25 ml per minute 135 psig at a flow rate of 0 5 ml per min ute and 275 psig at a flow rate of 1 0 ml per minute 7 Limit the vertical fall of the outlet tubing as much as possi ble to reduce siphoning action 3 9 Noise Filter The UA 6 includes a built in noise filter with RISE TIME set tings of 0 5 1 5 and 5 0 seconds RISE TIME is a response speed measurement defined as the time required to make a 1046 to 9096 pen deflection This filter can be used to reduce the noise level on the recorder trace It is especially useful for reducing or elimi nating flow noise caused by pulsatile pumps or noisy solvents see Figure 3 7 The figure demonstrates the ability of the noise filter to reduce baseline noise at 0 002 AUFS The filter used is an active Bessel filter Bessel filters are advan tageous because they merely delay rather than distort the shape of peaks This delay causes some increase in the response time of a peak and reduces the peak height of very short duration peaks but the peak areas remain constant 0 5 2 5 5 0 RISE TIME RISE TIME RISE TIME Figure 3 7 Effect of Noise Filter on Baseline Noise In many low pressure LC applications the 1 5 and 5 0 second set tings can be used to reduce baseline noise without any negative effect to the chromatogram M Note
33. must be taken not to scratch any of the optical surfaces of the quartz windows It is not likely that the regulator will become plugged However if it should become plugged remove the pressure regulator car tridge from its housing and place it in an ultrasonic cleaner using 6M nitric acid and then distilled water for ten minutes in each The regulator should then be thoroughly flushed with distilled water or methanol If you have a problem with the instrument or need parts infor mation contact Teledyne Isco s Service Department If you write please include all pertinent information that may be helpful in solving your problem Address your letter to Teledyne Isco Service Department Box 82531 Lincoln NE 68501 We suggest you call the Service Department first however before deciding to return the unit for factory repair Often a problem can be solved in the field with just a little extra help Our toll free number is 1 800 775 2965 Be sure all parts and hardware are back in place before packing Wrap the unit in heavy paper or put it in a plastic bag If the original shipping carton is not available put the wrapped unit in a strong cardboard box at least six inches longer in each basic dimension than the unit Fill the box equally around the unit with resilient packing material shredded paper bubble pack expanded foam chunks etc Seal it with strapping tape or gummed cloth tape and ship it to the address given previo
34. of the reading The AUTO BASELINE function can be activated by an external controller also Apply a TTL low or contact closure across pins 1 and 9 common of the fraction collector con nector 2 7 6 Detector Section 2 Preparation for Use 2 8 UA 6 Detector Section 3 Operation 3 1 Introduction The basic operation of the UA 6 consists of selecting the settings for sensitivity noise filtering peak separation if applicable and the built in chart recorder Once the flow cells and filters have been selected and installed the following steps should be fol lowed for starting operation 1 Move the STANDBY OPERATE switch to the OPERATE position With a Type 11 optical unit The LED will be red for the first 10 minutes of operation After 10 minutes the LED will change to green indicating the lamp current is set and ready for operation Should the LED change back to red during operation the lamp current may require adjustment See Section 4 for adjusting lamp current M Note Under normal conditions the LED should not change from green to red An ambient temperature change of more than 15 C or a weak lamp are generally the cause of lamp current to go out of regu lation After an intermittent power loss if the UA 6 power LED does not return to green see Section 4 for adjusting lamp current Should the UA 6 power LED flicker red green this indi cates the 1140 lamp is also flickering See Table 5 1 Sect
35. the position of the 50 or 60 hertz jumper P105 is fed into two dif ferent clock inputs of U104 One of the clock pulses is inverted by U107B so U104A will clock on the positive going edge and U104B will clock on the negative going edge This will create a 90 phase shift between the output of U104A and U104B The pulse train alternately turns on the four pairs of source drivers U101 to run the stepper motor B1 The pen is driven by a cord attached to a pulley The pulley is gear driven by a DC motor The pulley is attached to a potenti ometer R1 to provide feedback on the pen s position U102A is a voltage follower which buffers the incoming signal U102B then compares the input voltage to the position of the feedback poten tiometer R1 The positive or negative resultant output voltage then turns on either Q101 or Q102 to run the servo motor B2 The motor runs in the proper direction until the pen and feedback potentiometer are in the correct position 4 7 6 Detector Section 4 Theory of Operation 4 3 Type 11 Optical Unit This section explains the optical unit theory of operation To Theory of Operation provide a clear basic understanding of the optical unit circuitry equivalent circuits and mechanical functional diagrams are used in the following paragraphs An equivalent circuit is a simple electronic symbol which is used in place of the detailed circuitry but still maintains identical terminal characteristics of the de
36. the detector control system and system repair replace using the procedures specified in Section 4 2 Unstable or noisy a The lamp current is not set correctly a Some lamps while operating at a given cur baseline rent become unstable or develop a step char acteristic as observed on the recorder Change lamp current by moving S401 in the UA 6 5 16 6 Detector Section 5 Maintenance and Adjustment Table 5 5 Type 11 Optical Unit Troubleshooting Continued Problem 3 Slower than normal response Probable Cause b No flow cell in the optical unit REFER ENCE CELL B light path c UV lamp in the optical unit is unstable during coldroom operation d UV lamp in the optical unit is unstable e Condensation on the flow cell windows f Liquid is leaking across the flow cell win dows g Temperature fluctuations in the coldroom at temperatures below 10 C h Draft or air currents are hitting the optical unit Fluctuations are more noticeable in the higher sensitivity ranges 0 002 0 005 0 01 0 02 0 05 i Regulating photocell assembly is defec tive Usually indicated by not being able to adjust the lamp current correctly j When operating the optical unit in the 0 002 0 005 0 01 0 02 0 05 ranges noise and drift are reflected in the indications k Fluctuations in pressure or flow rate through the flow cell are causing noise and drift problems Noticeable when using
37. the procedure in Section 5 1 6 Detector Section 5 Maintenance and Adjustment RECORDER TIMING BELT SIDE PLATE MOTOR SPROCKET MOTOR MOUNTING SCREWS Figure 5 3 Timing Belt Tension Adjustment 5 4 Cleaning the Enclosures 5 5 Troubleshooting To clean the enclosures of the UA 6 and the optical units use a mild detergent in water For stains of an organic nature use iso propyl alcohol in a sponge that has been mostly squeezed dry The following sections identify the most common malfunctions that may occur during normal operation of the detector These tables identify the most commonly found problems and their causes and remedies A separate table is provided for each of the detector main systems or functions 5 5 6 Detector Section 5 Maintenance and Adjustment N DANGER Risk of electric shock Disconnect the electric power before servicing Only trained service personnel may remove the case top Table 5 1 Baseline Troubleshooting 1 No baseline adjust ment when using the Type 11 optical unit 2 Auto baseline does not bring chart pen on scale a The source screen and filter assemblies are not matched sets b When two different wavelengths are in use there may be a difference in relative brightness c The detector has not been correctly cali brated d INTERNAL EXTERNAL recorder switch set to EXTERNAL e Incorrect adjustment of the optical unit BASELINE ADJUST
38. up to several 68 0080 023 liters per minute The cell has a 1 8 inch bore flow path to allow fast flow rates with a minimum of back pressure The cell has a 5 mm pathlength 3 3 Flow Cell Descriptions For certain applications it may be necessary to change the O ring in your flow cells for increased solvent resistance Use the solvent compatibility chart Table 3 1 to determine which O ring will best suit your application requirements For a free guide to solvent compatibilities order a copy of Teledyne Isco Tables Table 3 1 O Ring Solvent Compatibility Chart Chem ER won Acids concentrated or Dilute Excellent Excellent Excellent Acid Inorganic Excellent Good Good Excellent Acid Organic concentrated Excellent Fair Good Poor Good Dilute Excellent Excellent Good Excellent Acid Oxidizing Concentrated Excellent Poor Good Dilute Excellent Good Excellent Alcohols Excellent Good Excellent Fair Excellent Alkalies Concentrated Excellent Excellent Poor Dilute Excellent Excellent Chlorinated Hydrocarbons Good Poor Ethers Excellent Fair Halogenated Solvents Poor Poor Good Excellent Hydrocarbons Aliphatic Excellent Poor Excellent Hydrocarbons Aromatic Excellent Good Excellent Excellent Ketones Excellent Good Excellent Poor Source Chemical resistance Guide for Elastomers Compass Publications 1988 3 2 6 Detector Section 3 Operation 3 3 1 Preparative FlowCells The preparative flow cells
39. 0 U211 8211 270 1900 06 U212 102 279 0022 00 206 U214 308A OR 070 212 1279 0403 00 0208 7555 371 2002 90 R202 RES 2 0M 1 4W 1 R258 6 CR201 CR202 CR203 CR204 CR205 CR206 CR207 CR209 CR210 CR211 19 402 0237 00 0201 0202 XSTR PNP 2N3702 20 221 222 430 0015 30 201 THMS 15 1 8W 10x PTC 223 60 0225 006 0216 SEL 60 0945 026 C231 C233 CAP MATCHED PAIR 227 120 0015 00 FL201 FL202 FL203 FL204 FL205 FILTER EMI 1000pF FL206 FL207 141 9000 24 J219 SKT 24 PIN RTANG 141 9002 01 J217 SKT 9 PIN D SUB RTANC NOTE This list subject to change without notice A 5 z e BB co NO 210 1 215 21 1 1 2 dd IN IN UA 6 Detector Appendix A Replacement Parts C408 P424 R403 O 58459
40. 1 5 mm FERRULE P N 60 0083 163 FERRULE INSTALLATION PROCEDURE Slide lead connector nut over tubing Slide ferrule over tubing For black lead connector with either 1 16 or 1 8 OD tubing insert tubing until it bottoms out on the lead connector For red lead connector with 1 8 OD tubing also insert tubing until it bottoms out For red lead connector with 1 16 OD tubing or beige lead connector with 1 8 OD tubing insert tubing through entire connector until it protrudes 1 8 beyond end of lead connector Slide ferrule into lead connector and secure with lead connector nut Trim excess tubing flush with end of lead connector CAUTION Do not overtighten lead connector nut Overtightening can lead to collapsing thin walled tubing 1 Red lead connectors have 0 063 1 5 mm fluid passages Black lead connectors have 0 036 0 9 mm fluid passages Beige lead connectors have 0 128 3 0 mm fluid passages 2 Tubing OD tolerance is 2 mm Figure 3 6 Ferrule Application Information 6 Detector Section 3 Operation 3 7 2 Flow Rate 3 7 3 Preparative Cells 3 8 Avoiding Bubble 3 10 Formation and Retention The Teledyne Isco high flow rate cell is designed to handle liquid flows up to about 3 liters min with negligible pressure drop Liquids with viscosities much greater than water may present difficulties at high flow rates while most cells can handle higher flow rates of water or other non viscous liquids if some pressure
41. 2 1 6 2 4 6 1 0 005 0 8 2 0 6 0 0 01 0 58 18 5 8 0 02 0 52 1 7 5 7 0 05 2 0 0 5 1 5 5 0 4 2 5 Recorder Offset Set Lamp and Optics 4 2 6 Peak Separation 4 2 7 Injection and Event Mark 4 2 8 Lamp Brightness Regulator UA 6 Detector Section 4 Theory of Operation U215B performs five functions Reduces the signal from the noise filter from 1 53 at full scale to 1 0 V Provides 86 of scale recorder offset in conjunction with R01 Ties the event mark signal to the recorder signal Ties the inject mark signal to the recorder signal When the sensitivity range switch is set on SET LAMP amp OPTICS and the optical unit is properly balanced U215B works in conjunction with Q204 U213A and 505 to offset the recorder signal to 0 of scale U215D offsets and amplifies the noise filter signal for the peak separator The peak separator U401 and U404 outputs a signal that is proportional to the edge slope or time derivative of a detected peak A fast slope causes the output of U404B to be greater than a slow slope The PEAK DURATION switch S506 compensates for this fact by making the detector more sensitive for slow peaks TP402 will give a reading between 0 and 8 5 V for negative peak edges and a reading between 0 and 8 5 V for pos itive peak edges Operational amplifier U404D switches from 13 V to 13 V when a negative edge is detected Operational amplifier U404C switches from 13 V to 13 V when a
42. 200 300 400 500 600 700 800 900 1000 FLOW RATE FLOW RATE mI MIN m MIN PREPARATIVE FLOW CELLS PREPARATIVE FLOW CELLS 20 imm 5 5mm E PATH v ER LENGTH SUCROSE WATER SUCROSE v 3 PRESSURE PRESSURE J PSI PS EH 2 e 52 I I i I 20 40 60 80 100 500 1000 1500 2000 2500 3000 FLOW RATE FLOW RATE ml MIN PREPARATIVE FLOW CELLS HIGH FLOW RATE FLOW CELL Figure 3 3 Flow Cell Flow Pressure Characteristics 3 5 6 Detector Section 3 Operation 3 4 Flow Pressure 3 5 Tubing Connections 3 6 Characteristics for Plastic Lead Connectors Refer to Figure 3 3 for flow versus pressure characteristics of Teledyne Isco flow cells M Note 1 Flow rate vs pressure drop characteristics were compiled using the lead connector that is packaged with each flow cell on the inlet port and no lead connector on the outlet port For the variable pathlength high flow rate flow cell the tubing connector for 1 4 and 3 8 inch OD tubing was used rather than the lead connector it is packaged with 2 The fluid temperature was 26 C for both water and sucrose solutions The medium pressure black and red plastic lead connectors are used with the preparative series 0080 001 0080 002 derated to 200 psi 14 kg cm flow cells These lead connectors should be used with s or 16 inch OD plastic or steel tubing with the fol lowing procedure see Figures 3 4 3 5 and
43. 7 400 0158 17 CR2 CR3 CR4 CR5 SHOTTKY DIODE 1N5817 9 402 0237 00 Q7 Q8 XSTR 2N3702 0 XSTR 2N6107 1 21 402 0262 92 0 XSTR 2 6292 22 402 0964 00 02 05 04 06 XSTR IRF9641 NO E 4 EN E Ez 995 1 This list subject to change without notice UA 6 Detector Appendix A Replacement Parts REVISIONS 92316 93011 033011 BY CHKD DATE 65 VPP 04001 JDD DESCRIPTION DESCRIPTION OF ITEMS 4 14 ITEM 7 WAS 180 0259 00 ADD ITEM 36 WHICH WAS ITEM 7 ADDED NOTE 2 AND ITEM 45 REMOVED ITEMS 6 14 17 26 92 260 030681 110196 CHG AUTHORITY A X XX XXX SHEET METAL 00 OTHER MATL 20 30 SURFACE ROUGHNESS 125 5 MAXIMUM Isco Inc LINCOLN NEBRASKA i2 THIS DRAWING PREPARED DRAWN BAC ACCORDANCE WITH 91155 ANSI ASME 14 5 1982 91162 SCALE 1 2 APPROVED 91162 REPLACEMENT PARTS LIST TYPE 11 OPTICAL UNIT 13348 T 30 LI0O tr11 09 N UNLESS PHOTOCELLS ARE INSTALLED AND CALIBRATED AT NOTES IT IS SUGGESTED IF PHOTOCELLS NEED REPLACING THAT THE OPTICAL UNIT BE RETURNED TO THE FACTORY THE FACTORY THE ACCURACY OF THE UNIT MAY NOT FALL VEN JANUARY 2004 ISCO COULD NO LONGER PURCHASE THE WITHIN THE STATED SPECIFICAT
44. 7 will double the cm ml Refer to Section 5 of the Tris manual for top removal and the circuit board location of P104 The actual chart speed cm hr when generating charts can be calculated from the following equation Tris speed x Tris range x UA 6 chart speed range x 0 049804867 UA 6 line frequency chart speed 0 to 10096 1 or 10 50 or 60 Hz Example 10096 X 10 300 cm hr 60 Hz 100 X 10 X 1 X 300 X 0 049804867 60 249 02343 cm hr Example 2596 X 1 15 cm hr 50 Hz 25 X 1 X 1 X 15 X 0 049804867 50 0 3735153 cm hr vii TELEDYNE ISCO RESEARCH AND APPLICATION LABORATORY The staff of Teledyne Isco s Research and Applications Laboratory is available to assist scientists in realizing and utilizing the full research potential of Teledyne Isco Instru ments When an application problem arises contact the laboratory director for assis tance Our staff will do its utmost in analyzing and solving any problems If you have developed a unique application for a Teledyne Isco Instrument or are considering a new use we would be interested in learning about it TRADEMARKS Amphenol is a Registered Trademark of BTC Electronic Components Halar is a Registered Trademark of Allied Corporation Hastelloy C is a Registered Trademark of Cabot Corporation Chemraz is a Registered Trademark of Venitron Corporation Locktite is a Registered Trademark of Loctite Corporation viii COMMONLY ORDERED REPLACEMENT PARTS FOR TH
45. AUFS on the 0 5 sensitivity range Observe precautions in Section 5 1 M Note The UA 6 was calibrated at the factory such that any optical unit can be connected to it and the accuracy of the system maintained But when field adjusting R224 the UA 6 will only be accurate with the optical unit with which it was calibrated Figure 2 5 Installing Flow Cells 2 8 Baseline Adjustment For baseline adjustment when starting operation set the UA 6 for Absorbance controls as follows 1 The PEAK SEPARATOR switch to OFF 2 The CHART SPEED selector to OFF 3 The STANDBY OPERATE switch to OPERATE 4 Allow a minimum of 15 minutes warm up to stabilize lamp current 5 Set UA 6 to SET LAMP amp OPTICS 6 Set the BASELINE ADJUST control to MAX open 2 6 10 11 6 Detector Section 2 Preparation for Use Adjust the BASELINE ADJUST control of the optical unit until the chart pen moves to near zero Ifthe indication from the previous step cannot be obtained turn the BASELINE ADJUST control of the optical unit to maximum open Move sensitivity switch off of SET LAMP amp OPTICS to desired absorbance range Align RECORDER OFFSET control to it s mark Activate AUTO BASELINE The pen should deflect near mid scale The baseline setting may be left at mid scale or moved to any arbitrary baseline by using the recorder offset control of the UA 6 Positioning the baseline will not alter the accuracy
46. E TELEDYNE ISCO UA 6 These replacement parts are often ordered by UA 6 owners All parts are pictured and identified by number and description in Appendix A Replacement Parts in the back of this manual Description UV lamp Hg vapor for Type 11 optical unit chart paper pens flow cell windows prep cell 10 mm diameter Type 11 filters 254 nm 280 nm Type 11 source screens 254 nm 280 nm flow cell connectors right lamp reflector left lamp reflector flow cell ferrules for 1 16 tubing Replacement lamps are tested to meet specifications Bubbles mer cury spots etc within the quartz envelope are not detrimental to the function of the lamp Part Number 60 0947 027 69 0943 193 68 0947 020 60 0644 052 60 1144 001 60 1144 002 60 1144 065 60 1144 008 68 1844 173 60 1143 049 60 1143 050 68 0084 014 5 UA 6 Table of Contents Section 1 Introduction 1 1 Optical Units for the 6 1 1 qaa ue s Sue Tet ae 1 1 1 2 Applications for the 6 1 2 1 2 1 Liquid Chromatography 1 2 1 2 2 Cuvette Reading 1 2 1 3 Technical Specifications 1 2 1 4 Controls and Indicators 1 2 Section 2 Preparation for Use
47. ENSITIVITY GREEN RED AUTO BASELINE PEAK SLOPE ae Ao AVERAGE PEAK OFF 300 DURATION MIN CHART SPEED PEAK SEPARATOR L Figure 1 2 UA 6 Front Panel LJ Table 1 2 Front Panel Controls and Indicators Switch STANDBY OPERATE 2 position selector switch In OPERATE applies secondary power to the unit In STANDBY applies secondary power to heaters When unit is connected to the main power source primary power 100 117 or 234 VAC is present at all times RECORDER Strip chart recorder Traces on graduated chart paper to indicate and record the light absorbency of a medium in the optical unit light path off 0 3 1 3 10 30 PEAK SEPARATOR Rotary selector switch Turns peak separator on optimizes the peak sepa rator for various peak widths in minutes 0 3 0 6 1 5 3 6 15 30 60 150 300 CHART SPEED CM HR Rotary selector switch Stops and starts recorder chart drive and selects speed ranges from 0 3 to 300 cm hr PEAK SLOPE LED Indicator lamp Lights green to indicate positive slope detected Lights red to indicate negative slope detected AUTO BASELINE Momentary push button Used to activate baseline circuitry Provide rapid coarse baseline adjustment 1 5 UA 6 Detector Section 1 Introduction Table 1 2 Eront Panel Controls and Indicators Continued SENSITIVITY 0 002 0 005 0 01 0 02 0 05 0 1 0 2
48. Figures 3 1 and 3 2 consist of a body fabricated from a fluoroplastic Halar two optically polished quartz windows and a lead connector screwed into each end of the body All preparative cells are equipped with lead connectors for 1 16 inch or 1 8 inch O D plastic or steel tubing A liquid tight seal is maintained by an O ring located between the quartz windows and the window nuts The cell is shipped with a round aperture in place Operation with the included optional rectan gular aperture is recommended when maximum resolution of small volume peaks is required If the rectangular aperture is used make certain the slit is aligned so it is perpendicular to the flow The lead connectors are fabricated from the same fluoroplastic the nuts are fabricated from an acetal plastic and the s inch 3 2 mm ferrule and 1 16 inch 1 5 mm ferrule are fabricated from polyethylene The combination provides the connection to either steel or plastic tubing Preparative flow cells are fabri cated with the light pathlengths specified in Table 3 2 Low Pressure Lead Connector Direction of Flow lt Body Window Window Nut PREPARATIVE FLOW CELL Figure 3 1 Preparative Flow Cell 3 3 6 Detector Section 3 Operation EFFLUENT OUT WINDOW WINDOW NUT ILLUMINATED VOLUME APERTURE O RING 7 LEAD CONNECTOR EFFLUENT PREPARATIVE FLOW CELL Figure 3 2 Flow Cell Cross Section Table 3 2 Flow Cell
49. IONS IDENTIFY WHICH BULB TYPE YOU HAVE AND ORDER ACCORDINGLY ORIGINAL BALL ENVELOPE BULB A 13 UA 6 Detector Appendix A Replacement Parts REPLACEMENT PARTS LIST 60 1142 017 5 2 OF 2 5 Inc REV E DATE 033011 M PART NUMBER DESCRIPTION 60 0995 005 PHOTOCELL MATCHED PAIR 60 0994 005 REGULATING PHOTOCELL ASSY 60 1145 052 KNOB za om 60 1144 065 254 NM SOURCE SCREEN 60 1144 008 280 310 SOURCE SCREEN 60 1144 001 254 NM FILTER 60 1144 002 280 NM FILTER 60 1145 022 TOP PLATE RETAINER 2 z TELTET MERC NU s mE mE mE si mE EN s s Note 1 For current prices and quotations on parts contact Isco Service Department 800 228 4250 2 This list is subject to change without notice UA 6 Detector Appendix A Replacement Parts UA 6 Detector Appendix A Replacement Parts REPLACEMENT PARTS LIST 00 2142 010 SHEET 2 OF 5 Isco Inc REV B 91241 tee PART NUMBER DESCRIPTION 140 0107 00 CABLE MOUNT PLUG 400 2152 14 DIO 1N5231B 60 1314 037 PHOTOCELL HOLDER 60 0995 005 PHOTOCELL MATCHED PAIR UNLESS PHOTOCELLS ARE INSTALLED AND UNIT CALIBRATED AT THE FACTORY THE ACCURACY OF THE UNIT MAY NOT FALL WITHIN THE STATED SPECIFICATIONS IT IS SUGGESTED IF THE PHOTOCELLS NEED REPLACING THAT THE OPTICAL UNIT BE RETURNED TO THE FACTORY 7 60 1145 001 8 60 2144 002 APERTURE PLATE ASSY 10 60 2147 021 ZINC LAMP CASSETTE AS
50. OURS L INSTRUMENTATION D ISCO AVEC PRUDENCE ET SENS COMMUN AVIS Si vous employez cet instrument d une autre que celles qui sont specifi es dans ce manuel la protection fournie par l instrument peut tre affaiblie Cela augmentera votre risque de blessure ADDENDUM The chart recorder of the UA 6 can be set to produce charts based on cm ml length of chart per unit vol ume pumped instead of the traditional cm hr length of chart per unit time For volume based charts plug the square 4 pin connector on the cable part number 60 1020 163 or 60 1020 228 into the socket labeled REMOTE CHART DRIVE on the rear panel of the UA 6 The chart length per unit volume cm ml is shown on the table below for each chart speed setting on the UA 6 the tubing size in the TRIS pump and line frequency 60 Hz in the USA 50 Hz in Europe etc CHART LENGTH PER UNIT VOLUME PUMPED Approximate cm ml FOR SINGLE CHANNEL OF PUMP Chan Speed 60 Hz Line Frequency 50 Hz Line Frequency cm hr 1 16 tubing 1 8 tubing 1 16 tubing 1 8 tubing 300 1 7 0 5 2 0 0 6 150 0 83 0 25 1 0 0 3 60 0 33 0 1 0 4 0 12 30 0 17 0 05 0 2 0 06 15 0 083 0 025 0 1 0 03 6 0 033 0 01 0 04 0 012 3 0 017 0 005 0 02 0 006 1 5 0 0083 0 0025 0 01 0 003 0 6 0 0033 0 001 0 004 0 0012 0 3 0 0017 0 0005 0 002 0 0006 M Note Changing the jumper in the Tris pump from the default setting P104 pin 4 8 to P104 pin 3
51. PTICAL LOGARITHMIC INVERTING UNIT AMPLIFIER AMPLIFIER CONFIG OUIPUI Figure 4 5 11 Absorbance Detector Block Diagram UA 6 Detector Section 4 Theory of Operation 4 12 UA 6 Detector Section 5 Maintenance and Adjustment 5 1 Removal and Installation of the Case Top 5 2 Part Replacement 5 2 1 Recorder Replacement This section presents the maintenance procedures that may be required in the field These procedures may be performed without the use of specialized equipment The procedures are limited to the replacement of specific parts and troubleshooting the detector For problems more serious than those listed contact Teledyne Isco s Service Department for help NDANGER Risk of electric shock Disconnect the electric power before servicing Only trained service personnel may remove the case top S Earth ground bonding connector Do not remove or disconnect Remove the four case top screws two screws on each side of the case Slide case top up and off The following paragraphs provide instructions for replacement of parts requiring specific procedures The majority of replacement parts require soldering When removing electronic parts with multiple leads each lead should be labeled for identification prior to being disconnected Ensure that capacitors diodes and transistors are installed in the correct positions and where applicable with the correct polarity Replace the recorder us
52. REW LAMP SOCKET SCREWS 2 2 HINGED ASSEMBLY SCREW 20F4 CENTER TOP PLATE SUB ASSEMBLY REFLECTORPLA TES PHOTOCELL ENDPLA TE FILTER HOLDER 1962 ASSEMBLY 192 10F2 SET SCREW Figure 5 4 UV Lamp and Regulating Photocell Removal and Installation 5 14 ASSEMBLY ADJUSTMENT SCREWS 7 REGULATING PHOTOCELL UVLAMP REGULATINGPHOT OCELL 4 MOUNTING ASSEMBLY 5 6 3 Filter Assembly Inspection 5 6 4 Troubleshooting UA 6 Detector Section 5 Maintenance and Adjustment If the optical unit malfunctions and the possible cause is a defective filter assembly Figure 5 4 it is possible to visually check the filter assembly using the correct light source intended for the wavelength involved The 405 nm through 660 nm filter assemblies can be checked by using an ordinary visible light source Fluorescent light is recommended for the 405 nm through 620 nm filter assemblies incandescent light source for the 660 nm filter assembly N WARNING Do not expose the naked eye to the UV light inside the optical unit Common clear eye glasses will provide adequate protection providing the UV light cannot reach the eye tissue without passing through the glass lenses UV light can damage the eye tissue even from side angle exposure without looking directly at the source The filter assembly should be removed
53. SY 11 60 2147 020 CADMIUM LAMP CASSETTE 12 60 2147 022 MERCURY LAMP CASSETTE ASSY 13 60 2144 015 214 FILTER 15 144 026 LTER 1144 002 LT 308NM FILT 310 340NM FILT 326NM FILTER 1144 006 FILTER 1144 021 ER 60 2144 022 M FILTER 60 2144 027 546 FILTER 26 60 1144 025 579 580 FILTER 28 60 2144 020 643NM FILTER 29 60 1144 070 SCREW ASSY 30 60 2144 028 SCREW ASSY 69 2145 0035 TRANSFORMER Note 1 For current prices and quotations on parts contact Isco Service Department 800 228 4250 2 This list is subject to change without notice UA 6 Detector Appendix A Replacement Parts REPLACEMENT PARTS LIST wo 80 2142 01 SHEET 3 OF 5 Isco Inc REV B DATE 91241 PART NUMBER DESCRIPTION 180 0259 00 KNOB W POINTER 1 For current prices and quotations on parts contact Isco Service Department 800 228 4250 2 This list is subject to change without notice UA 6 Detector Appendix A Replacement Parts This page intentionally left blank UA 6 Detector Appendix A Replacement Parts 34 IO PIN LA Rigg 04 M RIS ECT TL C 7D 105 act 77 c HT R 1 RI DER 9 R J TPIO2 E 108 RIN UST R109 O RII2 JA eo 2 gt E 86 dex CRIOS ww fio m5 45 e
54. T 10MV CIRCUIT BREAKER PRIMARY POWER IS PRESENT IN THIS INSTRUMENT AT ALL TIMES ALWAYS UNPLUG THE INSTRUMENT FROM THE POWER OUTLET AND DISCONNECT ALL FLEXIBLE CORDS BEFORE REMOVING THE COVER OR MAKING REPAIRS APPRARATUS PROTECTED UNDER A sans A 2X af 1 5 0 Figure 1 3 UA 6 Rear Panel 1 6 M Note UA 6 Detector Section 1 Introduction There are fuses located on the circuit board that are not acces sible to the user They are F401 0 75 Amp type F F402 1 5 Amp type and F403 0 75 Amp type F Table 1 3 Rear Panel Controls and Connectors OPTICAL UNIT 24 pin Amphenol socket Connector for attaching a Teledyne Isco optical unit FRACTION COLLECTOR INPUT OUTPUT 9 pin Sub D Outputs Peak separation Peak duration Inputs Event mark INJECT Baseline mark Auto 3 pin male manufactured per recommenda tions 100 VAC 117 VAC or 234 VAC power supply input for the detector CIRCUIT BREAKER 1A 100 and 117 VAC 0 5A 234 VAC Resettable circuit breakers only one is installed for 100 or 117 volt operation Limits the detector current drawn from the main power supply Push to reset RECORDER SELECTOR 2 position slide switch Selects signal source for UA 6 recorder INT Operates from UA 6 absorbance signal EXT Recorder o
55. T PARTS LIST NO 60 0082 046 SHEET 2 O 2 REV 6 DATE 98168 PART NUMBER DESCRIPTION 60 0644 052 QUARTZ WINDOW 1 2 3 60 0645 254 INSERT 69 0085 004 FLOW CELL WRENCH 60 0645 254 60 1844 175 CONNECTOR PACKAGE INCLUDES ITEMS 4 6 810 4 5 6 7 60 0925 015 60 0645 270 1 INSERT 202 5070 15 O RING VITON 60 0085 159 WINDOW 60 0084 014 FERRULE PACKAGE 025 0504 02 065 ID X 1 8 OD TUBING 025 0504 01 TFE TUBING 022 ID X 1125 OD 60 1844 176 CONNECTOR PACKAGE INCLUDES ITEMS 6 10 amp 14 60 0923 013 CONNECTOR 15 025 0502 04 1 030 ID X 063 OD TUBING 16 202 9074 26 0 RING CHEMRAZ 22 NOTE 1 This list is subject to change without notice UA 6 Detector Appendix A Replacement Parts HIGH FLOW RATE FLOW CELL Fixed Path Length 68 0080 023 Drawing modified 7 6 11 to remove obsolete flow cells A 23 UA 6 Detector Appendix A Replacement Parts REPLACEMENT PARTS LIST NO 60 0052 046 SHEET 2 2 REV DATE 95311 Mo PART NUMBER DESCRIPTION _ p _ 6 60 0084 014 FERRULE PACKAGE 8 60 1844 175 CONNECTOR PACKAGE INCLUDES ITEMS 6 9 amp 13 9 60 0925 015 CONNECTOR NUT S 4 7 j j j j j j
56. aximum sensitivity is 0 002 absorption units full scale AUFS with ten ranges up to 2 0 absorption units UA 6 detector consists of two components the detector with built in chart recorder variable noise filter and peak separator and separated by a six foot cable one of two optical units The optical units house the lamp filters and flow cells and are designed to be plugged into the UA 6 and attached to a ring stand mast or shelf The Type 11 optical unit is the standard absorbance optical unit for detection at 254 and 280 nm with eleven optional wave lengths to 660 nm A mercury vapor lamp is used for all wave lengths 1 1 UA 6 Detector Section 1 Introduction e LE Figure 1 1 UA 6 Detector with Type 11 Optical Unit 1 2 Applications for the UA 6 1 2 Liquid The UA 6 is designed for chromatographic detection for low Chromatography pressure classical LC and high flow LC flow rates up to 3liters minute 1 2 2 Cuvette Reading The UA 6 can operate as a UV VIS computing colorimeter with optional cuvette holders and 10 mm cuvettes 1 3 Technical The technical specifications of the UA 6 are listed in Table 1 1 Specifications 1 4 Controls and The controls and indicators utilized in the operation of the UA 6 Indicators are illustrated in Figures 1 2 and 1 3 and described in Tables 1 2 and 1 3 UA 6 Detector Section 1 Introduction Table 1 1 Technical Specifications for the UA 6 Dimensions and Weight Dete
57. cations for the 6 1 3 1 2 Front Panel Controls and Indicators 1 5 1 3 Rear Panel Controls and Connectors 1 7 1 4 11 Controls and Connectors 1 8 2 1 Selectable Wavelengths for Type 11 Optical Unit 2 4 3 1 O Ring Solvent Compatibility 3 2 3 2 Flow Cell Specifications 3 4 3 3 Interface Cables 3 16 5 1 Baseline 5 6 5 2 Recorder Troubleshooting 5 8 5 3 General Troubleshooting 5 10 5 4 Filter Assembly Inspection 5 16 5 5 Type 11 Optical Unit Troubleshooting 5 16 5 6 Flow Cell Troubleshooting 5 20 xiii Isco UA 6 Table of Contents UA 6 Detector Section 1 Introduction 1 1 Optical Units for the UA 6 1 1 1 Type 11 The UA 6 detector is a photometric detector used to measure absorbance It is a dual beam dual flow cell fixed wavelength detector with interchangeable wavelength filters for absorbance detection from 214 to 660 nm M
58. ctor cabinet only Width 11 2 in 28 4 cm Height 6 5 in 16 5 cm Depth 13 0 in 33 0 cm Weight 14 6 Ib 6 6 kg Power Requirements Mains voltage line cord is a disconnect device Factory Set 100 VAC 10 VAC 0 4 Amps 117 VAC 10 VAC 0 4 Amps 234 VAC 23 VAC 0 2 Amps Line Frequencies 50 Hz or 60 Hz field convertible Power Consumption maximum 50 watts 117 VAC 60 Hz Type 11 Ambient Temperature Range 0 to 40 C Humidity 5 to 25 C 0 to 100 relative humidity maximum with heaters ON Type 11 and 12 optical unit 10 to 40 C 0 to 95 relative humidity maximum with heaters OFF Type 11 and 12 optical unit Full Scale Absorbance Linearity 0 002 0 005 0 01 0 02 0 05 0 1 0 2 0 5 1 0 2 0 Absorbance Units Full Scale AUFS 1 5 of full scale maximum deviation measured at mid point of 2 0 absorbance range Noise Specifications for the Type 11 Optical Unit Accuracy Relative 10 x 10 AU 280 nm 10 x 10 AU 254 nm Reference 8 x 109 ASTM All noise specifications are for 9596 total trace with dry PREP flow cells and 1 5 second RISE TIME setting reference 1 5 cm hr chart speed 3 of full scale all ranges Range to Range Tracking 2 of reading Noise Filter Stability baseline drift after 8 hour warm up at constant ambient temperature Bessel time delay type Selectable 0 5 1 5 and 5 0 seconds RISE TIME setting
59. d pulley Make one revolution clockwise around the hub and route it up through hole E and secure it to the spring Leave enough tension so that the spring extends about 1 millime ter M Note You may find it difficult to secure the string to the spring while maintaining a slight tension If so secure the string to the spring then loosen the machine screw B and draw the ten sion from that end of the string Then retighten screw B 11 Install the T shaped stop bracket removed in step 1 and rotate the hub counter clockwise until the trapezoidal stop is against the stop bracket 12 Complete the string installation by threading the pen holder screw A back through the washers Be sure the washer with the string through it is in the middle Then tighten the screw to retain the string to the pen holder when the pen is slightly above full scale 100 1 Remove the case following the procedure in Section 5 1 2 Loosen two screws securing the motor mounting bracket to the side plate of the recorder Removal of main circuit boards may be necessary unless a right angle offset screwdriver is used to loosen motor screws 3 Slide the motor bracket back to increase tension on the timing belt and tighten the two screws N CAUTION Do not apply too much tension to the timing belt The timing belt should just be tight enough to ensure that the teeth do not jump out of the sprocket depressions 4 Install the case following
60. drive the optical unit and prepare its light sensitive signals to be recorded on a chart All current UA 6 optical units are dual light path devices which use two flow cells as depicted in Figure 4 1 The optical units all operate with a single light source which emits the desired ultra violet and visible spectrum When this light is passed through the two flow cells it interacts with the liquid There the light is changed by the absorbing nature of the liquid and its contents Then it is filtered so only the desired wavelength s are passed on to the photo detectors Electric currents are generated by the detectors which are proportional to the light intensity falling on them These currents are passed to the detector where they are recorded and used to control other analytical equipment SCREEN REFERENCE FLOW CELL REFERENCE FLOW CELL MEASURING REFERENCE PHOTOCELL R PHOTOCELL N gt o I a FILTER FILTER PHOTO CELL 4 1 6 Detector Section 4 Theory of Operation 4 1 2 UA 6 Detector OPTICAL LOGARITHMIC COMPENSATION OUTPUT AMPLIFIER C AMPLIFIER The detector presented as a block diagram in Figure 4 2 receives two current signals from the optical unit These two signals are subtracted from one another In general one signal is generated by a reference liquid most likely a non sample injected buffer If both light paths are buffered with the
61. drop across the flow cell is not objectionable In principle flow rates can be as high as that which does not result in a pressure drop exceeding the rated pressure limit of either the flow cell or fittings However an excess of pressure drop across the flow cell requires higher total pressure for the chromatographic system which may present difficulty for some chromatographic pumps With 60 aqueous sucrose solutions at 800 ml min as an example of a viscous liquid 58 cP UA 6 preparative cells show about 6 psi pressure drop With water at 50 ml min the prepar ative cells show about 2 psi pressure UA 6 preparative flow cells can often be applied in experiments where flow rates exceed 1 liter min At extremely low flow rates e g below 10 ml hr preparative flow cells are recommended because of their better gas bubble expelling properties At very low flow bubble problems will be increased because of greater increased heating of the eluent as it passes through the detector In low pressure liquid chromatography where the peak volume of eluted components is large over 1 ml preparative flow cells are best These cells have a straight through vertical flow design to quickly expel trapped bubbles due to outgassing The larger illu minated volumes of preparative flow cells do not affect the intensity resolution or the shape of larger peaks Bubbles form in a flow cell when it is warmer than the temper ature of the column and becau
62. e system and use another type e g Teledyne Isco precision metering syringe pump or install a pulsation damper in the flow system I Adjust the UV lamp using the procedures Section 5 6 1 step 11 Adjust the regulating photocell using the procedures in Section 5 6 2 If required bend or trim the reflectors m Return optical unit to Teledyne Isco for photocell replacement a Replace the UV lamp using the procedures specified in Section 5 6 1 b Check the filter using the procedures speci fied in Section 5 6 3 c Return optical unit to Teledyne Isco for pho tocell replacement d Replace the source screen 5 17 UA 6 Detector Section 5 Maintenance and Adjustment 5 7 Flow Cell The following paragraphs present maintenance procedures that Maintenance and may be required in the field These maintenance procedures are Adjustment limited to replacement of specific parts and troubleshooting without the requirement of special equipment 5 7 1 Window or O Ring Replacement of windows or O rings for all flow cells except the Replacement variable pathlength see Section 5 7 3 is presented in the fol lowing sections Replace the windows or O rings using the fol lowing procedure Refer to Figure 5 5 1 Using the special window nut wrench supplied carefully unscrew the window nut from the flow cell body Use the large end of the wrench for the preparative flow cell win dow nuts Remove the aperture inser
63. e RIIS a R 121 sa SE XL Res RII9 Glos Z Q A EE MAIN BOARD 8206 UA 6 Detector Appendix A Replacement Parts REPLACEMENT PART LIST Isco Inc MAIN CIRCUIT BOARD REV B DWG NO 60 2142 019 SHEET 5 OF 5 DATE 91241 112 5050 00 102 DESCRIPTION CAP 10uF 20VDC 112 3522 00 107 108 22uF 15VDC 400 0816 00 400 2147 14 101 102 104 105 CR103 CR1 DIO MR816 DIO 1N4764 400 2152 16 CR107 CR1 DIO 1N5261B 401 0150 00 108 DIO 1N5060 400 0914 00 402 1000 50 109 1 0101 0102 DIO 1 914 XSTR TIP50 402 0237 02 0103 0104 0105 XSTR 2 353707 402 0237 03 0106 XSTR 2 353710 380 1305 41 R117 POT 50 OHM 1 2W 270 0406 00 0101 5525 1 For current prices and quotations parts contact Isco Service Department 800 228 4250 2 This list is subject to change without notice A 20 UA 6 Detector Appendix A Replacement Parts PREPARATIVE FLOW CELLS 68 0080 001 68 0080 034 68 0080 002 60 0082 044 G PREPARATIVE FLOW CELL REPLACEMENT PARTS FOR REPLACEMENT PARTS SEE PARTS LIST DRAWING NUMBER 60 0082 046 FLOW CELL BODY Drawing modified 7 6 11 to remove obsolete flow cells A 21 UA 6 Detector Appendix A Replacement Parts REPLACEMEN
64. e one source screen and one metal blank of the same size Loosen the thumbscrew and replace the source screen with the slide matching the new wavelength selected Place the new source screen and the metal blank in the slide holder and tighten the thumbscrew Return the source screen holder to the slot in the Type 11 Figure 2 4 Changing the Source Screen in the Type 11 Optical Unit 2 6 Installation of Flow Cells M Note Always connect flow cells so that the direction of flow is up Select the correct flow cell for your application see Section 3 2 Using the two white latches on the front open the optical unit and install the flow cells into the reference and measuring com partments as shown in Figure 2 5 If the reference cell is left dry as recommended it is not necessary that the two flow cells used be of identical pathlengths or even equal cell types It is recom mended that the UA 6 always be operated with flow cells in both reference and measuring compartments Do not operate without a flow cell in the reference compartment 2 5 6 Detector Section 2 Preparation for Use 2 7 Calibrating to an As a cross check an external standard solution can be used to External Standard calibrate the UA 6 Baseline unit at zero Prepare a solution of potassium chromate Use a 0 45 AUFS dilution Place the external standard solution in measuring cell A and 0 05 N KOH in reference cell B Adjust internal control R224 for 0 45
65. ed both photocells receive 12 V As the register advances one photocell is driven toward 18 V and the other toward 6 V depending on the direction the register counts The direction the register counts is based on the value of the absorbance signal The circuit will continue to operate until the voltages received by the logarithmic amplifier U214 are bal anced and the absorbance signal at TP208 is at zero volts As TP208 nears zero volts U205A or B will shift the frequency of U208 from the initial rate of 400 Hz to 80 Hz Once TP208 reaches zero volts U205C and D will signal the flip flop U209B and C latching it The circuit will continue to operate about five more seconds due to the delay created by C223 and R255 The delay is necessary to allow for system settling and to allow the chart pen to come on scale should the rise time filter be in the 5 0 second position Once the Auto Baseline circuit has latched the voltage to the optical unit photocells the voltage will remain constant The circuit will not become active until signaled again by the user 4 3 6 Detector Section 4 Theory of Operation 4 4 4 2 2 Logarithmic Amplifier 4 2 3 Gain Amplifiers 4 2 4 Noise Filtering M Note Auto Baseline repeatability varies depending on the sensitivity range used The following lists a few examples of Auto Base line repeatability Sensitivity Range Repeatability 0 002 25 of chart 0 02 3 of chart 0 2 0 2 of cha
66. ed in place of or in conjunction with those shown Table 3 3 Interface Cables Instrumentation Part Number of Cable Fraction Collectors Foxy R1 or R2 69 2134 173 Retriever 500 60 1020 217 ISCO UA 6 tube change DETESTOR FRACTION 1 COLLECTOR event mark integrator recorder signals signals DIGITAL inject chart EXTERNAL INTEGRATOR mork drive RECORDER CONTROLLER Figure 3 10 Input and Output Signals of the UA 6 3 16 6 Detector Section 3 Operation 3 13 1 Foxy R1 and R2 Cable 69 2134 173 should be used to connect a Teledyne Isco Fraction Collectors Foxy R1 or R2 to the UA 6 for level sensing slope detection and tube change event marks Figure 3 11 This cable has two con nectors at the UA 6 end allowing interface to the recorder output a dual banana plug or for peak separator input a 9 pin plug It is recommended that the UA 6 peak detector be switched to OFF and the Foxy R1 R2 peak separator be used instead Be sure the polarity of the black dual banana plug connector is correct Match the ridge or keel on the connector with the negative binding post on the detector FOXY R1 R2 REAR PANEL CONNECTORS UA 6 DECTECTOR CABLE 69 2134 173 Figure 3 11 Cable Connection to the Foxy R1 or R2 3 17 6 Detector Section 3 Operation 3 13 2 Teledyne Isco Use cable 60 1020 217 to connect the UA 6 with a Teledyne Isco
67. emblies is applied to two photodetectors which generate an electrical resistance that is inversely propor tional to the amount of light projected onto the photosensitive surfaces Any increase in the light intensity results in a decrease in the electrical resistance generated by the photodetectors Outputs from the photo detectors are transmitted to an absor bance detector control system which reflects these photodetector outputs as units of absorbance SPACER SOURCE SCREEN LIGHT SOURCE NORMAL LOCATION OF ELEMENT LIGHT SOURCE ELEMENT APERTURE PLATE ASSEMBLY FLOW CELL FLOW CELL MEASUREMENT CELL MEASUREMENT CELL B PHOTODETECTOR PHOTODETECTOR FILTER ASSEMBLY Wami UV LIGHT SOURCE FILTER ASSEMBLY REFLECTOR REGULATING a PHOTO CELL Figure 4 3 Type 11 Optical Unit Functional Diagram With respect to the 254 nm 280 nm 310 nm and 340 nm filter assemblies the UV lamp produces numerous discrete emission lines with a very prominent one at 254 nm The fluorescence filter assembly which is located in the light path after the light has passed through the flow cell consist of these main elements e A UV transmitting filter that blocks green visible light e A fluorescent layer that produces green fluorescence when excited by UV light Green transmitting filter 4 9 6 Detector Section 4 Theory of Operation The third element is unique to the Teledyne Isco fluorescence filter asse
68. equate protection providing the UV light cannot reach the eye tissue without passing through the glass lenses UV light can damage the eye tissue even from side angle exposure without looking directly at the source WARNING The lamp contains a minute quantity of mercury which is a hazardous substance Dispose of properly in accordance with local and federal statutes A broken lamp should also be cleared from the area in accordance with local and federal statutes La lampe dans la cassette contient une tr s petite quantit de mercure ou de cadmium selon le type de lampe ces substances sont consid r es comme toxiques Veuillez vous conformer la l gislation en vigueur en particulier en cas de destruction de la lampe pour le nettoyage ventuel des zones souill es et la r cup ration ventuelle de la lampe ou de ses d bris 1 Position the optical unit so that the plastic draw catches are nearest you then release the two plastic draw catches and open the optical unit to the fullest extent 2 Remove the source screen 3 Remove the four screws securing the center top plate sub assembly to the center bottom plate sub assembly and hinge end plate 4 Grasp the center top plate sub assembly and gently pull toward you lifting the leading edge at the same time N CAUTION Do not touch inside surfaces of reflectors with fingers as oil deposits from the skin will be baked on the special UV reflect ing surface resul
69. ery stable voltages to the optical unit photocells The LM369D is specified to 10 V 10 mV and tem perature drift of 0 3 mV C U212 provides the reference and sta bility for the 10 V regulator U210A CR208 The 10 V is also used to provide stable voltage to the optical unit photocells The description of the chart recorder can be broken into two func tional sections the pen drive and the chart paper drive The schematic available online should be referred to for the fol lowing circuitry descriptions The paper is advanced by a stepping motor connected with a belt to the paper drive sprockets The incoming ac line frequency of 50 or 60 hertz is shaped by U108 and then divided by U105 and U106 to advance the stepper U105 U106 and dual BCD binary coded decimal up counters The incoming line frequency is divided by 2 4 10 20 40 and 100 by U106 and additionally by 200 400 and 1000 by one counter in U105 The chart speed selector switch is used to connect the counter output for the desired chart speed to the other counter in U105 This counter divides by 5 or 6 depending on the position of the jumper P106 connected to pin 1 of U108A When operating on 60 hertz U108D and U107D provide 3 count high 3 count low 50 duty cycle pulse train to operate the stepper For 50 hertz operation U108B and U107C create a 21 2 count high 2 2 count low 50 duty cycle pulse train This pulse train output from U107C or U107D depending on
70. etting of the switch the peak separator may respond slightly slower in cutting the leading edge of the peak For peaks greater than 2X the selected setting of the switch the ending cut may be slightly early resulting in a certain loss of peak material Ideally the PEAK SEPARATOR switch should be set such that the peak width of all important peaks in the chromatogram are greater than 0 2 yet less than 2 times the setting of the switch 254 nm we PEAK WIDTHS in minutes 5 front 0 02 AU 3 0 6 k 4 5 6 an Injection 1 Mark 3 11 2 The Indicator LED 3 12 Performance and Use 3 12 1 Minimizing Trace Noise and Drift UA 6 Detector Section 3 Operation In practice nearly all peaks will be adequately separated unless the peak duration setting is grossly incorrect for example a setting of 30 MIN for a chromatogram with one minute peaks or vice versa The example in Figure 3 8 shows a chromatogram in which peaks were cut with one minute peak duration setting Note that all five peaks are adequately cut The peak separator can control a fraction collector It will advance the fraction collector to the next tube at the start of a peak and again at the end of the peak or in the case of Foxy send a peak signal for the duration of the peak When the absorbance changes from zero slope the baseline to positive slope leading edge of the peak the change is sensed by the peak separator circui
71. ew O ring flow cell windows b Window nut is loose b Using the special window nut wrench sup plied Figure 5 5 tighten the window nut until it is snugged down If not items a or b above a sealant is c Apply fluorosilicone oil using the proce required dures specified in Section 5 7 2 2 Leakage around the Lead connector is loose in the flow cell a For medium pressure lead connectors lead connectors or body loosen the nut and retighten the lead con nuts nector and nut using the procedures speci fied in Section 3 5 b Nut is loose on the lead connector b For medium pressure lead connectors tighten the nut using the procedures speci fied in Section 3 5 c Ferrule and or tubing is deformed c Disconnect tubing from the lead connector and cut off defective part For medium pressure lead connectors install a new ferrule and reconnect using the procedures specified in Section 3 5 d O ring between the lead connector and d Disconnect the tubing and remove the the flow cell body is defective The prepara lead connector Install a new O ring tive flow cell requires no O ring when fluoro carbon lead connectors are used For medium pressure lead connectors install the lead connector and tighten the nut using the procedures specified in Section 3 5 3 Bubbles the flow a Flow cell is dirty a Clean the flow cell using the procedures cell specified in section 5 7 4 b Liquids re
72. gative to zero slope inflection Event Mark Inputs Recorder Event Mark Display Open collector or contact closure Type Five to 10 full scale spike added to recorder signal Indication Downscale for fraction collector index upscale for accessory e g Foxy rack change Duration 1 2 second Maximum Altitudes Pollution Degree Installation Category 2 000 Meters Built In Recorder Chart Width 10 cm calibrated in fifth cm minor divisions Chart Speed 0 3 0 6 1 5 3 6 15 30 60 150 and 300 cm hr Chart Paper Length 3 000 cm roll Pen Lift manual External Chart Drive Control contact closure across pins 1 and 2 of rear panel connection stops the recorder chart drive External Chart Speed Control 300 cm hr and slower Operating Wavelengths of Optical Units Type 11 254 280 310 340 365 405 435 470 510 546 580 620 or 660 nm wavelengths Injection Marks 1 4 Input to allow externally activated injection mark to be placed on the recorder Activated by open collector or contact closure UA 6 Detector Section 1 Introduction UA 6 UV VIS DETECTOR TELEDYNE ISCO POWER LAMP GREEN OPERATE IF RED AFTER WARM UP RESET LAMP RED WARM UP OPERATE 0515 50 OT 9 RISE TIME SEC NOISE FILTER STANDBY 01 8 0 05 02 0 02 0 5 0 01 1 0 7 0 005 2 0 OPTIC RECORDER 000248 S
73. hs withthe from 254 to 660 nm with interchangeable filters and corre Type 11 Optical Unit sponding source screens see Table 2 1 The two wavelength filters selected must be of the same wavelength and must match the source screen used When the UA 6 and Type 11 are shipped filter and source screen for 254 nm are in place Figure 2 3 Changing Wavelengths in the Type 11 Optical Unit Table 2 1 Selectable WOODEN for Type 11 Optical Unit Wavelength nm Bandwidth nm Source Screen Light Source Spectral line ca 0 1 15 280 280 310 25 310 340 280 310 20 310 340 340 365 20 365 340 365 12 405 405 Spectral line ca 0 1 435 435 20 470 10 510 Spectral line ca 0 1 546 10 580 11 620 12 660 To change wavelength operation 1 Release the two white catches on the front of the unit and open the Type 11 and remove the wavelength filters from each side of the optical unit as shown in Figure 2 3 The BASELINE ADJUST control on the optical unit will have to be used to clear the access to the filter Remove the fil 2 4 UA 6 Detector Section 2 Preparation for Use ters by pulling gently Take care not to drop them they are breakable Press the selected filters in place and return the BASE LINE ADJUST control to its previous position Close the optical unit Select the source screen that matches the filters chosen Remove the source screen holder as shown in Figure 2 4 The source screen holder will hav
74. in each reflector Transverse openings in the flow cells provide a path for the light through an absorbing medium by intersecting longitudinal openings in the flow cell which provide the path for the absorbing medium The spatial integrating action of the elliptical reflectors and the translucent diffusing action of the source screen light source area produce extremely good optical balance between MEASURING CELL A and REFERENCE CELL B light paths This results in a very low recorder noise and drift regardless of the spatial or angular fluctuations in the light emitted from the UV lamp This important feature patent no U S 3 822 097 3 859 539 other patents pending contributes to the Type 11 optical unit s high performance Light radiating through the reflector aperture to the reference flow cell is interrupted by the aperture plate assembly once it has passed through the flow cell The aperture plate assembly con tains a teardrop shaped aperture that controls the amount of light passed on to the filter assembly and photodetector This pro vides a coarse baseline adjustment during calibration proce dures 4 8 UA 6 Detector Section 4 Theory of Operation Light radiating through the reflector aperture then through the measuring flow cell is filtered and passed to a photodetector Both filter assemblies which are matched in wavelength to the source screen transmit a narrow spectral region The resultant output from the filter ass
75. ing the following procedure see Figure 5 1 1 Remove the case top using the procedure in Section 5 1 2 Disconnect P102 on the recorder circuit board 3 Remove the recorder speed control connector P104 from the recorder circuit board 4 Remove the 3 nuts and washer securing the recorder to the detector front panel 5 Remove 1 screw from L bracket in rear top corner of the recorder 5 1 6 Detector Section 5 Maintenance and Adjustment 6 Remove 2 screws from case bottom 7 Remove 1 screw from the top left corner of the circuit boards it engages the recorder 8 Carefully remove the recorder from the detector N CAUTION Extreme care must be taken when removing the recorder not to damage any components within the detector 9 Carefully install the replacement recorder and all fasten ers previously removed 10 Connect P102 to the recorder circuit board 11 Insert the recorder speed control connector P104 onto the new recorder circuit board 12 Install the case top RECORDER RECORDER SECURING NUT WASHER si 1 OF 3 FRONT PANEL EN RECORDER SPEED A CONTROL CONNECTOR e 9 nor _ V POWER CONNECTOR TO UA 6 RECORDER SPEED CONTROL 2 4 A 7 Z Figure 5 1 Built In Recorder Removal and Installation 5 2 6 Detector Section 5 Maintenance and Adjustment 5 2 2 Recorder Drive String Read through the following instructio
76. ion 5 2 Select the sensitivity setting and allow the UA 6 to warm up until it stabilizes with solvent flowing through the cells For detection in 0 5 1 0 and 2 0 AUFS range a minimum of 15 minutes is needed For operation at the 0 005 or 0 002 AUFS ranges several hours of warm up may be required for stable operation 3 Baseline the detector see Section 2 8 4 Select the settings for the noise filter see Section 3 9 peak separator see Section 3 11 1 and chart speeds Uncap the chart pen and lower the pen onto the paper The UA 6 is now ready for operation 3 1 6 Detector Section 3 Operation 3 2 Flow Cell Applications The UA 6 has different types of flow cells for use with the Type 11 optical unit preparative cells for low pressure chromatography a high flow rate cell for LC with flow rates up to 3 liters per minute microcolumn for extremely small illuminated volumes and density gradient cells covered in a separate manual for scanning centrifuged gradients 3 2 1 Preparative FlowCells The preparative flow cells are designed for liquid column chro 68 0080 001 002 034 matography applications involving either low or high flow rates and large peak volumes The preparative flow cells have a straight through flow path that provides relative freedom from bubble problems but the large internal volume may cause a loss of resolution 3 2 2 High Flow Rate Cell This flow cell is designed for flow rates from 10 ml
77. ise is reduced 4 Reinstall the circuit board mounting screws case top and case top screws Drift performance is directly related to the stability of the ambient temperature The UA 6 can operate at any temperature between 0 C and 40 C without affecting drift as long as it remains stable Temperature changes of 1 C will cause noticeable drift at a SENSITIVITY setting of 0 002 AUFS Any step that tends to stabilize temperatures including insulating the system column tubing injection valve will help minimize drift Baffles to prevent drafts from room heating ducts from hitting the system are also helpful When operating in a coldroom the temperature may actually vary several degrees with the result that the baseline drifts accord ingly Baffling or insulating the optical unit from cooling fans that may cycle on and off intermittently can help limit drifting Solvent temperature may differ significantly from ambient tem perature As it moves closer to the ambient figure during the chromatographic elution baseline drift can sometimes be noted on the trace To correct this problem allow the solvent to come to ambient temperature prior to injection or equilibrate the column for a period of time to allow the trace to stabilize 6 Detector Section 3 Operation wu H15N313AVM 1201 0 7 uosyoer png s unos WU H15N313AVM 00 80070 9000 02070 08170 0 80 00071 aouequo
78. lowcell and fil ter for obstructions If the chart pen is near 100 of chart and can not be zeroed with the optical unit baseline adjust there is an obstruction in the measuring flowcell or filter Remove the obstruction a Turn the NOISE FILTER to reduce noise b Some lamps current becomes unstable or indicates a step characteristic as observed on the recorder Decrease the lamp current until the step characteristic disappears Do this by moving the internal jumper S401 inside the UA 6 c Install the same type of flow cell in the REFERENCE CELL B light path as in MEA SURING CELL A light path to improve the optical balance d Turn the COLDROOM HEATER switch to ON e Replace the UV lamp following the proce dure in Section 5 6 1 f For the Type 11 optical unit turn the COLDROOM HEATER switch to ON g Repair the leakage following the proce dure in Section 5 7 2 h Turn the COLDROOM HEATER switch to ON i Shield insulate or remove the optical unit from the air currents j Make allowances for the normal noise and drift refer to Table 1 1 Noise Specifications for detailed specifications k Increase the RISE TIME Remove the reciprocating pump from the system and use another type e g Teledyne Isco syringe pump or install a pulsation damper in the flow system 5 7 6 Detector Section 5 Maintenance and Adjustment N DANGER 1 Chart paper does not feed correctly Intermit
79. ly Replacement with the following procedure Figure 5 4 1 Position the optical unit so that the plastic draw catches are nearest you then release the two plastic draw catches and open the optical unit to the fullest extent 2 Remove the source screen 10 11 Remove the four assembly screws securing the center top plate sub assembly to the center bottom plate assembly and the hinged end plate Grasp the center top plate sub assembly and gently pull toward you lifting the leading edge at the same time Using a low wattage soldering iron disconnect the two wires to the regulating photocell assembly Snap the defective regulating photocell assembly out of the mounting assembly Snap the replacement regulating photocell assembly into the mounting assembly and using a low wattage soldering iron connect the two leads If required loosen the two photocell adjustment screws and adjust the mounting bracket to obtain 1 16 to 1 8 inch clearance between the end of the regulating photocell assembly and the UV lamp glass surface Replace the center top plate sub assembly The reflectors should have equal spacing on each side of the slot in the center bottom plate sub assembly so they are 3 16 inch apart and not touching the bulb at any point Install and tighten the assembly screws Install the source screen 5 13 UA 6 Detector Section 5 Maintenance and Adjustment ASSEMBLY SCREW 2 4 MOUNTINGCLAMP SC
80. m use a 1 or 2 mm cell 3 8 6 Detector Section 3 Operation Two types of very low density polyethylene ferrules are provided for use with this instrument Characteristic properties and application of these ferrules are as follows 1 16 inch 1 5 mm with ferrule P N 60 0083 163 OD OF TUBING TO BE USED 1 8 inch 3 2 mm with ferrule P N 60 0923 017 INSTALLATION PROCEDURE Finger tightening of connector nut Polyethylene ferrules may be used with acids bases and all organic solvents but are subject to long term damage due to swell when exposed to COMPATIBLE SOLVENTS halogenated hydrocarbons over extended time In most cases such a damaged ferrule is still useable until the lead connector nut is loosened unless the pressure of swelling collapses thin walled connecting tubing FERRULES PICTURED AS INSTALLED LEAD CONNECTOR NUT P N 60 0923 015 BLACK LEAD CONNECTOR P N 60 0923 013 1 8 inch TUBING 1 8 inch 3 2 mm FERRULE P N 60 0923 017 BEIGE LEAD CONNECTOR P N 60 1853 034 LEAD CONNECTOR NUT P N 60 0923 015 1 8 inch TUBING TRIM TUBING FLUSH 1 8 inch 3 2 mm FERRULE P N 60 0923 017 BLACK LEAD CONNECTOR LEAD CONNECTOR NUT P N 60 0923 013 P N 60 0923 015 1 16 inch TUBING 1 16 inch 1 5 mm FERRULE P N 60 0083 163 RED LEAD CONNECTOR P N 60 0643 254 LEAD CONNECTOR NUT P N 60 0923 015 1 16 inch TUBING TRIM TUBING FLUSH 1 16 inch
81. mation Customer Service Phone 800 228 4373 USA Canada Mexico 402 464 0231 Outside North America Fax 402 465 3022 Email IscoCSR teledyne com Technical Support Phone Toll Free 866 298 6174 Samplers and Flow Meters Toll Free 800 775 2965 Syringe Pumps and Liquid Chromatography Email IscoService teledyne com Return equipment to 4700 Superior Street Lincoln NE 68504 1398 Other Correspondence Mail to P O Box 82531 Lincoln NE 68501 2531 Email IscoInfo teledyne com Revised September 2012 Warnings and Cautions The lightning flash and arrowhead within the triangle is a warning sign alerting you to dangerous voltage inside the product gt The exclamation point within the triangle is a warning sign alerting you to important instructions in this manual Symboles de S curit gt Ce symbole signale la pr sence d un danger d lectrocution gt Ce symbole signale l existence d instructions importantes relatives au produit dans ce manuel und Vorsichtshinweise Der gepfeilte Blitz im Dreieck ist ein Warnzeichen das Sie vor gef hrlichen Spannungen im Inneren des Produkts warnt gt Das Ausrufezeichen Dreieck ist ein Warnzeichen das Sie darauf aufmerksam macht wichtige Anleitungen zu diesem Handbuch geh ren Advertencias y Precauciones gt Esta se al
82. mbly and improves performance by blocking violet and red stray light that passes through the first element CONNECTORPINS 2 CHASSISGROUND REFERENCECELL MA TCHEDP AIR MEASURINGCELL LES REGULA TINGCELL MERCURY VAPORLAMP SELECTED 50 5W i EM 20 ON COLDROOM HEA TERSWITCH OFF 21 10 22 13 14 A THISRESISTORIS INSTALLED AT THE DISCRETIONOF CALIBRATION EITHERONEOR THE OTHERISUSED 11 17 18 Figure 4 4 Type 11 Optical Unit Schematic Diagram 4 3 2 Absorbance Detector Circuit 4 10 The optical unit resultant output signal is applied to a loga rithmic amplifier Figure 4 5 in the absorbance detector control system which in turn generates an output signal that is the loga rithm of the input signal from the optical unit This logarithmic amplifier output signal voltage is proportional to the optical density or light absorbance of medium placed in the optical unit light path When signals from the logarithmic amplifier are applied to a linear inverting amplifier configuration the signals are inverted and the resultant output is a voltage which is propor tional to the optical density of the medium in the light path Any of the output signals from the optical unit may be used to drive read out devices or other analytical instruments through circuit selections made on the absorbance detector control system UA 6 Detector Section 4 Theory of Operation OUTPUT AMPLIFIER LINEAR O
83. nance and Adjustment Table 5 1 Baseline Troubleshooting Continued Problem 3 Unstable or noisy baseline when using a Type 11 optical unit Table 5 2 item 4 Probable Cause b Optical unit has an imbalance greater than 0 5 absorbance units a Normal noise more noticeable on sensi tive ranges b Lamp current needs to be changed c No flow cell in the Type 11 optical unit REFERENCE CELL B light path refer to Section 2 6 d Unstable UV lamp in the optical unit dur ing coldroom operation e Unstable UV lamp in the optical unit f Condensation on the flow cell windows g Liquid leaking across the flow cell win dows h Temperature fluctuations in the coldroom at temperatures below 10 C i Draft or air currents hitting a Type 11 opti cal unit This is more noticeable in the more sensitive ranges 0 002 0 005 0 01 0 02 and 0 05 j When operating in the 0 002 0 005 0 01 0 02 and 0 05 ranges there is noise and drift k Fluctuations in pressure or flow rate through the flow cell causing noise and drift problems Noticeable when using reciprocat ing pump Solution b Set the UA 6 to SET LAMP amp OPTICS and adjust the baseline control on the optical unit until the chart pen zeros If the chart pen is below 0 of scale there is a problem with the reference side of the optical unit Move the baseline adjust aperture out of the light path and check the reference f
84. ns and refer to Figure 5 2 Installation to replace the recorder drive string 1 Loosen the two stop bracket securing screws and remove the T shaped stop bracket 2 Use a felt tipped pen to draw a realignment mark across the pulley and gear assembly hereafter referred to as the hub This mark ensures that the orientation of the shaft and the hub is maintained during reassembly STOP REALIGNMENT MARK SPRING PEN HOLDER F SMALL PULLEY 1 OF 2 Sap 9 DELRIN WASHERS 1 OF 3 STOP BRACKET SECURING SCREW 1 OF 2 STOP BRACKET 1 16 SET SCREW Cu N Figure 5 2 Recorder String Routing 5 3 6 Detector Section 5 Maintenance and Adjustment 5 3 Timing Belt Tension 5 4 Adjustment 3 Loosen the two 16 inch set screws which secure the hub to the metal shaft and lift the hub completely off the metal shaft Loosen the pen holder screw marked A in Figure 5 2 remove it and take off the first two of the three washers 5 Remove the old pieces of the drive string Secure one end of the new drive string under the screw marked B 7 Route the string through hole C and up through hole D 8 Place the hub back onto the metal shaft ensure that is 10 properly aligned and then tighten the two set screws Route the string 180 degrees counterclockwise note arrows in Figure 5 2 around the small pulley marked F Then route the string through a washer and around the secon
85. o Teledyne Isco and Teledyne Isco will pay surface transportation to return the repaired instrument to the customer Teledyne Isco will not pay air freight or customer s packing and crating charges This warranty does not cover loss damage or defects resulting from transportation between the customer s facility and the repair facility The warranty for any instrument is the one in effect on date of shipment The warranty period begins on the shipping date unless Teledyne Isco agrees in writing to a different date Excluded from this warranty are normal wear expendable items such as pH sensors charts ribbon lamps tubing and glassware fittings and wetted parts of valves and damage due to corrosion misuse accident or lack of proper maintenance This warranty does not cover products not sold under the Teledyne Isco trademark or for which any other warranty is specifically stated No item may be returned for warranty service without a return authorization number issued by Teledyne Isco This warranty is expressly in lieu of all other warranties and obligations and Teledyne Isco specifically disclaims any warranty of merchantability or fitness for a particular purpose The warrantor is Teledyne Isco 4700 Superior Lincoln NE 68504 U S A This warranty applies to the USA and countries where Teledyne Isco does not have an authorized dealer Customers in countries outside the USA where Teledyne Isco has an authorized dealer
86. or remedies are 1 Ensure that the flow cell is vertical and the effluent is moving upward through it 2 Use the shortest pathlength flow cell possible Larger pathlength flow cells have a greater volume which may decrease the resolution due to mixing in the flow path b It is assumed that the correct baseline is the average of the baseline on both sides of the peak Run the solvent through a flow cell in the REFERENCE CELL B light path This flow cell should have the same pathlength and should be operated at the same wave length as the flow cell in the MEASURING CELL A light path 5 9 6 Detector Section 5 Maintenance and Adjustment N DANGER Risk of electric shock Disconnect the electric power before servicing Only trained service personnel may remove the case top Table 5 3 General Troubleshooting Problem Probable Cause Solution 1 Slower than normal response 2 Lamp flickers or UA 6 power LED stays red with a Type 11 opti cal unit connected 3 Automatic Peak Sep arator will not cause an Isco Fraction Collector to operate a Weak UV lamp in the optical unit b Defective optical unit filter c Defective fluorescent or diffusing light source slide d Defective photocells in the optical unit a Defective UV lamp in the optical unit or misalignment of lamp regulating photocell b Defective electronic components a Defective components in the detector Even
87. ore yellow c Same as item a d Same as item a d Same as item a Opaque e Cracks or deep pits f Violet f Cracks or dark spots g Deep blue g Same as item f h Blue h Same as item f i Deep green i Same as item f j Yellowish green j Same as item f k Yellow orange k Same as item f Red Same as item f m Deep red m Same as item f Table 5 5 Type 11 Optical Unit Troubleshooting Problem Probable Cause Solution 1 No baseline adjust a The source screen and filter assemblies Install the required source screens and ment are not matched sets matching filters see Table 2 1 b When two different wavelengths are in b Reverse the cell locations of the matched use there may be a difference in relative source screen and filter assemblies brightness c Flow cell is dirty c Clean the flow cell using the procedure specified in Section 5 7 4 d UV lamp in optical unit is defective d Replace the UV lamp using the procedures specified in Section 5 6 1 e The optical unit BASELINE ADJUST e Adjust using the procedures specified in rotary control is incorrectly adjusted Section 2 5 f Filter assembly in the optical unit is defec f Check the filter assembly using the proce tive dures specified in Section 5 6 3 g Defective photocell in the optical unit g Return the optical unit to Teledyne Isco for photocell replacement h Defective absorbance detector control h Check
88. ow Cells pathlengths are required for best performance and operation Generally you should select a flow cell with an illuminated volume no greater than about 10 of the smallest chromato graphic peak volume expected 3 7 1 Pathlength The best optical pathlength depends on the solute concentration and its absorptivity at the wavelength used As cell pathlength increases both signal and flow noise increase but instrument noise will remain the same Thus longer pathlengths give highest detectability For most purposes an intermediate pathlength is better because of smaller volume and in the case of preparative flow cells better liquid flow characteristics Nonlinear response due to detector bandwidth diminishes greatly as absorbance decreases Therefore photometric linearity can be improved with shorter pathlength cells which require high instrument sensitivities lower absorbance ranges for the same detectability This effect is particularly important when absorptivity of the compound varies over the wavelengths encompassed by the detector band width A UA 6 has a 0 1 nm bandwidth at 254 nm and certain other wavelengths which is excellent A UA 6 has a 15 nm bandwidth at 280 nm and certain other wavelengths which is only fair so shorter pathlength cells are generally better at these wave lengths For average applications use a 5 mm cell For very highly absorbing solutes or best quantitative accuracy with a UA 6 at 280 n
89. perates on an external 0 1V sig nal input RECORDER OUTPUTS 1 V 10 mV common ground chassis ground Banana sockets Connectors for an external voltage sensitive recorder INTERNAL RECORDER INPUT 1 V Banana sockets Input for operation of the UA 6 recorder from a separate 0 1V instrument INTEGRATOR REMOTE CHART DRIVE CONTROL Banana sockets 4 pin Jones plug For connection of external integrator computer Provides 1 volt per absorbance unit Connector for remote control of the built in recorder CHASSIS GROUND d Banana socket Connecting shield of I O cables to chassis SIGNAL COMMON v Banana socket Return for Digital Analog signal 1 7 UA 6 Detector Section 1 Introduction TA m 2 Figure 1 4 11 Controls Connectors Table 1 4 Type 11 Controls and Connectors Item in Detector Connect Cable Six individually shielded pairs Provides interface connection to with a 24 pin connector a Teledyne Isco absorbance detector control system BASELINE ADJUST MIN Rotary Control Moves an aperture plate assem OPEN MAX OPEN bly back and forth in the light path to meter the light for zero baseline calibration procedures COLDROOM HEATER ON OFF Toggle Switch SPDT Applies and removes approxi mately 13 VDC to the UV lamp and photodetector coldroom heaters SOURCE SCREEN HOLDER Holds source screen in place SECTION CLAMP Secures o
90. phy Flow Celis esos 3 8 9761 Pathlengthb usapu bu ee SN 3 8 3 2 Flow Rate 2 ne nen oh Sua Q ak ms 3 10 3 63 Preparative Cells lb up ei 3 10 3 8 Avoiding Bubble Formation and 3 10 3 9 Noise des an ee an eas DIES SEI 3 11 3 10 Built in Chart Recorder 3 12 3 11 Built In Peak 3 12 3 11 1 PEAK SEPARATOR Switch 3 12 8 1122 The Indicator LED user er ar wee 3 13 3 12 Performance and 4 3 13 3 12 1 Minimizing Trace Noise and Drift 3 13 3 12 2 Solvent Absorbance 3 16 3 13 Connection to Other Instruments 3 16 3 13 1 Foxy R1 and R2 Fraction Collectors 3 17 xi Isco UA 6 Table of Contents 3 13 2 Teledyne Isco Retriever 500 241245 an WEE ee sas 3 18 3 14 Remote Chart Drive Control by Non Isco Equipment 3 18 3 15 Converting the Internal Recorder for Stand Alone Operation 3 19 Section 4 Theory of Operation 4 1 4 2 4 3
91. positive edge is detected Capacitor C442 or C424 makes a pulse whenever U404D or U404C is turned on These pulses are used to index a fraction col lector when a new peak is detected or an old peak is finished U406A Q414 produce a peak duration signal TTL low to P107 J217 during a peak A positive spike can be placed on the chart recorder by shorting pin 4 to pin 9 of J217 the INJECTION MARK input This action will cause C232 to pass a pulse to operational amplifier U215C and then on to the recorder through the optical unit connector Pins 14 and 13 are shorted when the optical unit is plugged in The negative event mark spike works the same way when pins 3 and 9 of the FRACTION COLLECTOR connector are shorted together Here the pulse is made by C228 and operational amplifier U215A Located in the left center portion of the schematic this circuit is only active when UA 6 is used with a Type 11 optical unit When active it performs five functions 10 minute warm up cycle Limits lamp current to a maximum of 270 mA Automatically adjusts lamp current to a pre selected value Value is selected by user S401 Monitors lamp current Maintains lamp brightness 4 5 6 Detector Section 4 Theory of Operation When the UA 6 is switched to operate U403B begins to oscillate at a rate of 13 Hz Initially only U407 is clocked by U403B During the first 10 minutes of operation U403D limits the lamp current
92. ptical unit sides M Note Always leave the reference flow cell dry unless you are running a strongly absorbing gradient UA 6 Detector Section 2 Preparation for Use 2 1 Unpacking 2 2 Preparation for Use Power 2 3 Installing the Chart Paper and Pen Unpack the detector carefully Check all components and accessory packages against the packing lists Any damage or shortages should be reported immediately to Teledyne Isco Retain the shipping containers in the event the instrument needs to be returned to the factory for service Reference should be made to the warranty located in the back of this manual prior to assembling the instrument CAUTION Prior to connecting the UA 6 to power check the serial tag to ensure that the voltage and frequency requirements of the instrument are compatible with the available voltage and fre quency The UA 6 uses a detachable line cord Connect the receptacle end to the MAINS plug Figure 1 3 and then connect the plug to a properly rated mains supply To install the paper refer to Figure 2 1 1 Raise the pen lift arm so that the pen clears the roller 2 Unroll several inches of paper from a new roll of chart paper 3 Fold or cut the leading edge of the paper at a 30 angle Don t fold the paper into a point this tends to cause a snag 4 With the printed side of the paper away from you feed the paper up around the front of the paper guide and behind
93. quire degassing b Degas the liquids before they are entered into the system c Flow cell pressure is too low c Install restriction in the flow cell outlet line 5 7 4 Flow Cell Cleaning It is recommended that the flow cells and quartz windows or Procedures quartz rods for the variable pathlength be cleaned before the flow cell is used in a system To obtain the best cleaning results remove the quartz windows using the procedures specified in section 5 7 1 Purge the flow cell with a warm detergent solution and then rinse with distilled water or appropriate organic solution Oily deposits in a flow cell tend to aggravate the trapping of bubbles Rinse with a non polar solvent e g hexane followed by a rinse with a polar solvent e g methanol If the flow cell has been used with aqueous solutions precede the non polar and polar solvent rinses with an aqueous alkaline detergent solution rinse followed by a distilled water rinse then the polar solvent rinse This will usually remove contamination that causes bubble adhesion 5 20 5 7 5 Cleaning the Back Pressure Regulator 5 7 6 Service Department 5 7 7 How to Ship Returns UA 6 Detector Section 5 Maintenance and Adjustment To prevent a fungus growth after a flow cell has been used for density gradient fractionation with sucrose solution it is nec essary to either flush with alcohol or use an alkaline soap before the last distilled water rinse N CAUTION Extreme care
94. rcuit rotate the sensitivity switch S05 to SET LAMP amp OPTICS U402C will send a reset pulse to U403C and U405 Lamp current will change to 270 mA and slowly adjust down to the value selected by S401 Within 2 minutes the current should be set and the power LED green 4 2 9 Power Supply The UA 6 power supply has five voltage sources 24 VB unregu lated supplies power for optical unit lamps 24 V unregulated main 24 V source also provides power to 15 V regulator VRO1 15 V regulated by VR01 supplies power to all analog and digital circuitry VRO1 is a linear regulator 24 V unregulated only 24 V source also supplies power to 15 V regulator VR401 15 V regulated by VR401 supplies power to all analog and digital circuitry VR401 is a linear regulator When the UA 6 is connected to an AC power source and is in the standby mode three heater resistors R449 516 and 523 warm the unit This prevents moisture from condensing inside the unit should it be in a humid environment N CAUTION These resistors should not be touched when power is con nected to the UA 6 4 6 4 2 10 Built In Chart Recorder 4 2 11 Pen Drive UA 6 Detector Section 4 Theory of Operation In Operate mode normal circuit operation creates enough heat to prevent condensation In addition to the main power supplies there are 2 precision power supplies 10 V and 10 VDC U212 is a precision 10 V ref erence utilized to provide v
95. recip rocating pumps for high pressure in high speed chromatography in the 0 002 0 005 0 01 0 02 0 05 absorbance ranges Metal parts are touching the UV lamp glass surface this could be the regulating photocell assembly reflectors optical units with stamped metal reflector instead of the plated plastic reflector m Photocell in the MEASURING CELL and or REFERENCE CELLB light path is defective a UV lamp in the optical unit is weak b Optical unit filter is defective c Photocell is defective d Source screen is defective the light source is damaged Solution b Install the same type of flow cell in the REF ERENCE CELL B light path as that in the MEASURING CELL A light path to improve the optical balance The flow cell in REFER ENCE CELL B light path should be full of a clear bubble free liquid c Place the COLDROOM HEATER ON OFF switch to the ON position Figure 1 4 and Table 1 4 d Replace the UV lamp using the procedures specified in Section 5 6 1 e Same as item 2c above f Repair the leakage using the procedures specified in Section 5 7 2 g Same as item 2c above h Shield insulate or remove the optical unit from the air currents i Replace the regulating photocell assembly using the procedures in Section 5 6 2 j Make allowances for the normal noise and drift indications refer to Table 1 1 for detailed specifications k Remove the reciprocating pump from th
96. rt 0 5 2 0 Repeatable This circuit consists mainly of U214 amplifier U216 loga rithmic diodes and 9203 buffer The amplifier functions as common mode amplifier When both photocell signals are equal the output at TP208 is zero Therefore any system noise signals seen by both photocells are common moded out and not seen on the absorbance signal U213 is an adjustable amplifier used to compensate the response of optical units Resistors inside the optical unit increase or decrease the gain of this amplifier to maintain the amplification of the entire system regardless of the optical unit used The U213 amplifier couples the absorbance signal from the logarithmic amplifier to the absorbance amplifier Absorbance amplifier U202B provides the sensitivity ranges based on the front panel switch position S5B 0 002 range pro vides a gain of 100 Gain decreases to 0 1 on the 2 0 range The noise filter U202A is a Bessel type time delay filter whose output is the time average of its input Three filter settings are possible using S04 This filter will reduce the amount of system noise seen by the chart recorder lt 0 gt In addition to U202A the absorbance amplifier U202B provides filtering in the four most sensitive ranges The following infor mation relates total system rise time in seconds per sensi tivity rise time setting for a 10 90 of scale signal change Sensitivity Noise Filter Setting 0 5 1 5 5 0 0 00
97. s 10 to 90 full scale response Type 11 optical unit 2 x 10 AU maximum in 4 hours 254 or 280 nm wavelengths 4 x 103 AU maximum in 4 hours all wavelengths measured with dry prep flow cells and the same wavelength in both optical beams Recorder Outputs 0 to 1 V 1 into 100K ohms or greater 0 to 10 mV 1 into 1K ohms or greater Zero common mode voltage Recorder Input 1 V maximum internal recorder input Integrator Output 1 0 VDC Absorbance unit 3 of scale plus 2 of reading 1 3 UA 6 Detector Section 1 Introduction Table 1 1 Technical Specifications for the UA 6 Continued Peak Separator Peak Duration Ranges Example Long Duration Peak Short Duration Peak Maximum Slope Sensitivity 0 3 1 3 10 30 minutes One hour base width with a minimum height of 10 of scale 10 second base width with a minimum height of 4 of scale 0 0055 typical full scale per second positive slope 30 minutes peak width setting Sensitivity is inversely proportional to peak width setting Negative slope sensitivity is 1 5 times as great as positive slope sensitivity The sensitivity is reduced to 3 4 on the 0 01 range 2 on the 0 005 range and 1 4 on the 0 002 range to minimize detection of noise peaks Peak Separator for Fraction Collectors OPEN COLLECTOR Max V 30 VDC Max 0 5 ADC One second TTL low standard across pins 6 and 9 TTL low on zero to positive slope inflection and ne
98. s exigences du Reglement sur le mat riel brouilleur du Canada P Ra RB SERE VI s yu s BJ Name and amount of Hazardous Substances or Elements in the product HEN RMR SIE S ES Hazardous Substances or Elements Component Name En D TMB A WJ ZW RAS Pb He Cd Cr VD PBB PBDE FINEST O x O O O O UV Lamp z BAR x O O O O O Circuit Boards DO Dit BAL x O O O x O AC Motor I y BAL x x O DC Motor z Bx O O O O x O Wiring gt HY BUR O X Line Cord 3 x O O O x O Transformer Name and amount of Hazardous Substances or Elements in the product O k E P 8 O Represent the concentration of the hazardous substance in this component s any homogeneous pieces is lower than the ST standard limitation X AGRECB SERE ILS AR HST WENENRERR TEHA BYR IR ET HE 2b HLA X Represent the concentration of the hazardous substance in this component s at least one homogeneous piece is higher than the ST standard limitation Manufacturer may give technical reasons to the X marks EUR FH HB 101 The Environmentally Friendly Use Period EFUP was determined through experience FF ARREARS A WSUS AEH 207 520074 MAN SFARRAD A AF BA A 55
99. same substance any unwanted signal interference generated by the liquid e g tem perature drift optical density or refraction changes are reduced by this subtraction process thus making the system more stable The difference signal is converted to a logarithmic function The chart recorder output is the logarithm of the light intensity Next the signal is amplified and filtered as necessary At this point it is sent to the peak separation network and chart recorder With the help of any external signals that may be present like event marks from a fraction collector or injection marks from an auto matic injection valve a trace is made on the recorder chart paper The necessary control signals for indexing a fraction collector are also generated RE ER FRACTION COLLECTOR INJECTION AND EVENT MARKS Figure 4 2 UA 6 Detector Block Diagram 4 2 4 2 Detailed Description 4 2 1 Auto Baseline Circuit UA 6 Detector Section 4 Theory of Operation Refer to the UA 6 schematics available online during the fol lowing description To view the schematic drawings for the UA 6 first find the serial number for your unit Then go to our Web site at www isco com Select Service and then Fast Thorough Factory Repair Service The link to schematics is under Circuit Schematics After you enter your serial number you will be able to view the schematics online If you need any assistance or don t see the correct sche matic for
100. se the cross sectional area of the flow path is changing rapidly The following steps taken sepa rately or combined should deal with most bubble problems 1 Degas the buffer or solvent prior to eluting the column by applying a vacuum Heating or ultrasound treatment dur ing vacuum degassing is beneficial 2 Warm the buffer or solvent if possible to about 3 C above the column temperature This decreases the ability of the mobile phase to absorb and hold gases 3 Be sure the direction of flow through the flow cell is from bottom to top 4 Be sure the flow cells are clean Material from a previous application that coats the inside of a flow cell may provide a surface for bubble formation and adhesion Excellent cleaning results can usually be obtained by using isopropyl alcohol IPA water detergent solution water IPA hex ane IPA and finally water In some cases it may be neces sary to remove the flow cell windows and clean them separately see Section 5 6 2 5 Select the appropriate flow cell 6 Detector Section 3 Operation 6 Apply a back pressure on the flow cell by using a 100 psig back pressure regulator available from Teledyne Isco part number 209 9012 22 a long piece of small bore tubing or some other device on the outlet side of the flow cell Keep the column to flow cell tubing length as short as possible This is especially true for exclusion chromatography gel filtration because of its higher
101. sensitivities It is caused by a scattering of the light Filtering all of the components of the mobile phase to remove particulates is the best solution for this problem A 0 45 filter is adequate for almost all cases Static discharge may also cause noise problems when the humidity is very low The best way to circumvent this is not to touch the system while a chromatogram is running Baseline noise can be affected by the lamp in a Type 11 optical unit Generally a noisy lamp will produce wider baselines If a noisy lamp is suspected the lamp current should be changed 3 13 6 Detector Section Operation 3 14 N DANGER Risk of electric shock Disconnect the electric power before servicing Only trained service personnel may remove the case top 1 Disconnect the line cord Remove the two screws from each side of the case top Slide the case top off 2 Remove the two screws from the top of the circuit board power board on the right hand side of the instrument Fold the circuit board down exposing the component side of the board 3 Locate S401 selectable jumper on the power board near the adjacent circuit board toward the front of the instru ment Slide the selectable jumper off 5401 and move it to another position it is not critical which position is selected Each position provides a different current which will change the lamp characteristics If the baseline is still noisy move the jumper until the no
102. should contact their Teledyne Isco dealer for warranty service Before returning any instrument for repair please call fax or e mail the Teledyne Isco Service Department for instructions Many problems can often be diagnosed and corrected over the phone or by e mail without returning the instrument to the factory Instruments needing factory repair should be packed carefully and shipped to the attention of the service department Small non fragile items can be sent by insured parcel post PLEASE BE SURE TO ENCLOSE A NOTE EXPLAINING THE PROBLEM Shipping Address Teledyne Isco Attention Repair Service 4700 Superior Street Lincoln NE 68504 USA Mailing Address Teledyne Isco PO Box 82531 Lincoln NE 68501 USA 800 775 2965 lab instruments 866 298 6174 samplers amp flow meters Sales amp General Information 800 228 4373 USA amp Canada Phone Repair service Fax 402 465 3001 Email October 11 2013 P N 60 1002 040 Rev H IscoService teledyne com 236 TELEDYNE ISCO Everywhereyoulook
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104. t applicable only to the prepar ative flow cell Remove the O ring Carefully install the replacement window in the flow cell body M Note Refer to the Replacement Parts List in the back of this manual that is applicable to the flow cell in use to obtain the Teledyne Isco part numbers for the replacement items 5 Moisten the replacement O ring with distilled water and carefully install on top of the window Carefully install the aperture insert applicable only to the preparative flow cells on the window nut with the large outside diameter against the nut before assembly of the nut in the flow cell N CAUTION Use extreme care when performing step 7 Do not cross thread or over tighten the window nuts This can result in damage to the window and or window nuts and strip the threads in the flow cell body 7 5 18 Install the window nut and tighten with the special win dow nut wrench Use the large end of the wrench for the preparative flow cells Tighten the window nuts only until they are snugged down Install the flow cell in the system and check for leaks If there are any leaks around the windows perform the pro cedures specified in Section 5 7 2 UA 6 Detector Section 5 Maintenance and Adjustment WINDOW NUT WRENCH WINDOW NUT APERTURE APERTURE INSERT INSERT OPTIONAL STANDARD RECTANGULAR t ROUND O RING Preparative Flow Cells and Fixed Pathlength High Flow
105. t Mark circuitry b Incorrect connection to the fraction collec tor c The fraction collector is defective a Replace the UV lamp see Section 5 6 1 b Check the filter and if required replace it see Section 5 6 3 c Replace see item 7 Figure 5 4 d Return optical unit to Teledyne Isco for photocell replacement a Replace or realign the UV lamp see Sec tion 5 6 1 b Using standard electronic techniques repair or replace parts as required a Using standard electronic techniques repair or replace as required b Connect the detector to the fraction collec tor following the procedure in Section 3 13 c Check this out by shorting pins 6 and 9 on the detector end of the fraction collector cable while the cable is plugged into the frac tion collector This short should cause the fraction collector to index 5 6 11 Optical Unit Maintenance 5 6 1 Type 11 UV Lamp Replacement UA 6 Detector Section 5 Maintenance and Adjustment The following sections present the maintenance procedures that may be required in the field These maintenance procedures are limited to replacement of specific parts and troubleshooting without the requirement of a service person or special equipment Replace the optical unit UV lamp using the following procedure Figure 5 4 WARNING Do not expose the naked eye to the UV light inside the optical unit Common clear eye glasses will provide ad
106. tailed circuitry The theory of operation is presented at two levels in the following paragraphs The first level provides general data on the overall optical unit system and the second level provides information on specific individual system circuits 4 3 1 General The optical unit Figure 4 3 is an electro optical transducer that develops an electrical signal varying resistance in response to changes in sensed light levels The optical unit consists basically of a UV light source flow cells two reflectors a reference and measuring photocell two filter assemblies a regulating photocell assembly source screen and a baseline adjusting aperture plate assembly The UV light source is at one focus of an oblate spheroid ellipse of revolution formed by the two reflectors and the source screen is at the other focus resulting in almost total capture of radiation in the system When the same wavelength is used in both the MEASURING CELL A and REFERENCE CELL B light paths only one source screen is used UV light is reflected from the two reflectors and excites both sides of a light source which is part of the source screen resulting in a light emission spectrum at a certain wavelength region Depending upon the source screen used the emitted light is either diffused light from the UV lamp or is fluorescent light excited by the UV lamp This light emission spectrum is radiated from the source screens to the flow cells through an aperture
107. tent stoppage of the chart may be due to PROBABLE CAUSE a b or c Pen trace not parallel to printed chart lines may be due to PROBABLE CAUSE 2 Recorder does not write 3 Pen does not respond to absorbance changes 4 Erratic trace on the recorder chart Risk of electric shock Disconnect the electric power before servicing Only trained service personnel may remove the case top Table 5 2 Recorder Troubleshooting a Chart paper sprocket holes are not cor rectly mated to the recorder drive roll sprock ets b Timing belt tension not adjusted correctly c Motor drive sprocket not secured to the motor shaft a Ink cartridge empty b The pen manual lift arm is in the full up position a INT EXT recorder switch set to EXT b The recorder 192 tooth gear is not secured to the feedback potentiometer shaft c Pinion assembly is not secured to the DC motor shaft d Recorder servo string is loose or broken a Bubbles passing through the flow cell b Condensation on the flow cell windows c Leakage across the flow cell windows a Install the chart paper following the proce dure in Section 2 3 b Adjust the timing belt tension following the procedure in Section 5 3 step 3 c Tighten the motor drive sprocket set screw see Figure 5 3 a Replace the pen following the procedure in Section 2 3 b Place the pen manual lift arm in the full down position
108. ting in permanent damage and attenuation of the UV light Check the inside surfaces of the reflectors If the surfaces are dirty they should be replaced 5 Remove the defective UV lamp 6 Detector Section 5 Maintenance and Adjustment N CAUTION Do not handle the new UV lamp glass surfaces with bare hands Oil deposits from the skin will be baked on the UV lamp glass surfaces resulting in permanent attenuation of the UV light Clean the UV lamp glass surfaces with clean hexane then with a spectro quality methanol or equivalent to remove dirt or fingerprints 6 Carefully install the replacement UV lamp M Note It is strongly recommended that locally purchased UV lamp replacement not be used All lamps utilized in Teledyne Isco optical units are subjected to very stringent test procedures and approximately 50 are found to be unusable 7 Connect the optical unit absorbance detector and turn the unit ON 8 If required loosen the set screw and rotate the UV lamp socket until the bright spot in the UV lamp is facing directly up Tighten the set screw and turn the optical unit OFF 9 Replace the center top plate sub assembly The reflectors should have equal spacing on each side of the slot in the center bottom plate sub assembly so they 3 16 inch apart and not touching the bulb at any point 10 Install and tighten screws 11 Ifrequired loosen the two securing screws securing the UV lamp socket assembly
109. to 270 mA and the power LED will be red After approxi mately 10 minutes U407 pin 3 will go high producing the fol lowing results U403B will begin clocking 0405 U403A inhibits any further clocking of U407 U402D and Q405 shift the oscil lator frequency of U403B to about 500 Hz Now that U405 is being clocked the circuit will begin to adjust the lamp current to the value selected by S401 U405 performs two functions The three most significant bits adjust the fre quency of U403B progressively slower in 8 steps to around 50 Hz This helps maintain the rate of lamp current change since the amount of change per step increases as U405 advances its count U405 also adjusts lamp current by biasing U402B and the regu lating photocell in the optical unit As the lamp current decreases from 270 mA U402A will change the power LED to green and shift the frequency of U403B to around 1 Hz U403C monitors lamp current through R463 When the current through R463 matches that selected by S401 U403C will stop the oscillator U403B This latches the entire circuit Now the bias provided by U405 will remain fixed and the regulating photocell in the optical unit will maintain the lamp brightness Should the lamp current fall below 183 mA or exceed 260 mA after the 10 minute warm up cycle U402A will change the power LED from green to red This notifies the user that the lamp current is out of regulation and may require adjustment To rein itialize the ci
110. to the hinged end plate and move the UV lamp socket assembly to obtain clearance between the UV lamp and the reflector plates M Note The mounting clamp must be removed prior to loosening the two securing screws 12 Install a 254 nm source screen Holding a flow cell squarely in position turn the optical unit ON Sight through the flow cell and aperture in the UV lamp reflector plate Cen ter locate the UV lamp until a blue and red illuminated area is centrally positioned in the light path If required loosen the set screw to obtain the UV lamp position ensur ing that the bright spot is still facing directly up The UV lamp must not touch the reflector plates or the source screen 13 Tighten the two securing screws and if required the set screw Check to ensure that the blue and red illuminated area is still centrally positioned through the flow cell and light path aperture 5 12 14 15 16 6 Detector Section 5 Maintenance and Adjustment Turn the optical unit OFF If required loosen two photocell adjustment screws and adjust the regulating photocell to point at the UV lamp bright spot with a 1 16 to 1 8 inch clearance between the regulating photocell and the UV lamp glass surface Sighting through the flow cells check that the blue and red illuminated area is centered If not repeat steps 12 through 15 above 5 6 2 Regulating Photocell Replace the regulating photocell assembly P N 60 0994 005 Assemb
111. try This initiates a tube change signal to the fraction collector For a SLOPE the LED emits green light to show that the peak separator has sensed the rising slope of a peak When the maximum of the peak is detected zero slope the LED extinguishes When the trace starts down the trailing edge of the peak the LED emits red light When the absorbance reaches a minimum at the end of the peak this may be at a baseline different from the leading edge of the peak i e a shifted baseline the LED will extinguish the fraction collector will advance one position When used with fraction collectors that include a delay timer the peak separator can be used to precisely collect peaks by synchro nizing the action of the fraction collector with the actual arrival of the peak at the drop outlet When used with fraction collectors without a delay timer satisfactory peak cutting will occur but the fraction collector will move slightly prematurely at the beginning and end of the peak For peak cutting in low pressure LC this is seldom a problem This section covers generalized information on several aspects of the UA 6 that can help you use the instrument more effectively One source of noise is the solvent itself Certain organic solvents among them chloroform hexane and methanol are inherently noisy In the more sensitive ranges an alternative solvent may be advisable Noise from micro particles in the solvent may be noticeable at very high
112. usly The warranty at the end of the manual describes the conditions under which Teledyne Isco will pay surface shipping costs It is very important that the shipment be well packed and fully insured Damage claims must be settled between you and the carrier This can delay repair and return of the unit to you 5 21 UA 6 Detector Section 5 Maintenance and Adjustment 5 7 8 Purchasing Parts 5 22 Only the parts listed in the Replacement Parts List of this manual are stocked for immediate delivery by Teledyne Isco Vir tually all other parts are also available but there may be some delay in shipping them because they are not normally stocked The figures in the Replacement Parts section illustrate the immediate delivery items Each replacement part is given an item number which is shown in the callouts in the illustration and in the item number column of the list When ordering replacement parts please supply this information 1 series number of the unit 2 item number 3 part number UA 6 Detector Appendix A Replacement Parts A 1 Replacement Parts Replacement parts are called out in the following pages Refer to the call out in the adjacent table to determine the part number for the item Replacement parts can be purchased by contacting Teledyne Isco s Customer Service Department Teledyne Isco Customer Service Department P O Box 82531 Lincoln NE 68501 USA Phone 800 228 4373 402 464 0231 FAX
113. your specific unit contact our service department The Auto Baseline circuitry provides rapid coarse baseline adjustment Maximum adjustment time is ten seconds An optical unit with an imbalance as great as 0 5 absorbance units can be baselined by this circuit If an imbalance of greater than 0 5 absorbance units exists in the optical unit the circuit will continue to hunt until the imbalance is corrected by the operator When the UA 6 is switched to operate U211 generates a reset pulse 10mS width which centers the address register U201 203 and 204 With the address register centered U207 and U210 provide 12 VDC 0 5 V to each photocell in the optical unit By pressing the front panel push button switch S2 or applying a TTL low to pin 1 of the rear panel fraction collector connector J217 the Auto Baseline circuit is activated Oscillator U208 begins to clock the address register U201 203 204 up or down depending on the signal received from U205C and U205D U205C and U205D monitor the absorbance signal from the loga rithmic amplifier to determine which direction the circuit should count As the address register advances the voltage produced by the DAC U207 and buffer amplifier U210D U210B advances The measuring photocell in the optical unit is fed directly with this voltage The reference photocell however is fed by an inverted signal derived from the measuring photocell voltage When the address register is center

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